Automatic digestion device for iron sodium leaf green acid sample pretreatment

Abstract

The utility model provides an automatic digestion device for iron leaf green acid sodium sample pretreatment relates to digestion equipment technical field, including the reaction jar and the storage jar, the surface of reaction jar is equipped with the detector, the inside of reaction jar is equipped with the stirring subassembly, the bottom surface of storage jar is equipped with the communicating tube, the surface of communicating tube is equipped with the flow transducer, adopts three groups of storage jar, three detectors, flow transducer and first electric control valve, realizes the real -time monitoring to the digestion liquid multipoint through three detectors, including absorbance, conductivity, pH etc. parameter, the multi -parameter signal of three detectors of controller real -time acquisition, when the detector detects the digestion progress deviation, the controller instantaneous instruction corresponding first electric control valve opens or closes, and according to the feedback accurate metering of flow transducer three groups of storage jar in nitric acid, hydrogen peroxide and pure water's make -up, thereby dynamic adjustment of the proportion of input, avoid organic residue residue or iron ion excessive loss, finally the stability of iron recovery rate and batch -to -batch repeatability are improved significantly.

Description

Technical Field

[0001] This utility model relates to the field of digestion equipment technology, and in particular to an automatic digestion device for pretreatment of sodium iron chlorophyllate samples. Background Technology

[0002] Sodium iron chlorophyllin, an iron-rich green pigment derived from chlorophyll, is widely used in the food, pharmaceutical, and cosmetic industries. Its sample pretreatment digestion is a preliminary step in quality testing (such as iron content and heavy metal analysis). Existing technologies mainly employ wet digestion processes, including manual or semi-automatic hot plate heating, microwave-assisted digestion systems, and general-purpose automatic digestion systems. These systems are typically equipped with acid-resistant digestion tubes, peristaltic pump dispensing modules, programmable temperature-controlled heating plates, graphite furnaces or microwave cavities, exhaust gas absorption devices, and PLC control units. They support the oxidative decomposition of the nitric acid-hydrogen peroxide system. Through fixed-ratio addition of digesting agent, timed heating programs (pre-digestion at 120℃, main digestion at 180-200℃, and acid removal stage), and cooling to volume, the organic matrix is ​​destroyed and target ions are released. These systems are suitable for use in conjunction with atomic absorption spectroscopy or ICP analysis.

[0003] Currently, the existing pretreatment digestion process for sodium ferrochlorophyllin samples typically uses a fixed ratio of digesting agent, which cannot adapt to the significant differences in content between sample batches. This leads to excessive organic residues during under-digestion or excessive iron ion loss during over-digestion, resulting in large fluctuations in iron recovery rate and poor batch-to-batch repeatability. In addition, relying on manual experience to visually judge the digestion progress by color or bubbles is prone to subjective errors, and the order and amount of liquid added are difficult to control precisely. Utility Model Content

[0004] The purpose of this invention is to address the shortcomings of existing technologies by proposing an automatic digestion device for the pretreatment of sodium iron chlorophyllate samples.

[0005] To achieve the above objectives, the present invention adopts the following technical solution: an automatic digestion device for pretreatment of sodium ferrochlorophyllin samples, comprising a reaction vessel and a storage tank, wherein a detector is provided on the surface of the reaction vessel, a stirring assembly is provided inside the reaction vessel, a connecting pipe is provided on the bottom surface of the storage tank, a flow sensor is provided on the surface of the connecting pipe, a first electrically controlled valve is provided on the surface of the connecting pipe, a heating assembly is provided inside the reaction vessel, and a drain pipe is provided on the bottom surface of the reaction vessel.

[0006] Preferably, the stirring assembly includes a servo motor, a rotating rod, and a stirring rod, wherein the output end of the servo motor is provided with a rotating rod, and the surface of the rotating rod is provided with a stirring rod.

[0007] Preferably, the surface of the reaction vessel is provided with a controller, which is electrically connected to the detector and the first electrically controlled valve respectively.

[0008] Preferably, the top surface of the reaction vessel is provided with a first support leg, and the end of the first support leg is connected to the bottom surface of the storage tank.

[0009] Preferably, the top surface of the reaction vessel is provided with a guide pipe, and the surfaces of both the guide pipe and the drain pipe are provided with a second electrically controlled valve.

[0010] Preferably, the storage tank and connecting pipe are arranged in three groups in a circular array, and the detector is arranged in three groups in a circular array.

[0011] Preferably, the surface of the reaction vessel is provided with an exhaust pipe, and the bottom surface of the reaction vessel is provided with a second support leg.

[0012] Beneficial effects This invention employs three sets of storage tanks, three detectors, a flow sensor, and a first electrically controlled valve. The three detectors enable real-time multi-point monitoring of the digestion solution, including parameters such as absorbance, conductivity, and pH. The controller collects multi-parameter signals from the three detectors in real time. When a detector detects a deviation in the digestion progress, the controller immediately instructs the corresponding first electrically controlled valve to open or close. Based on feedback from the flow sensor, the controller precisely measures the amount of nitric acid, hydrogen peroxide, and pure water added to the three sets of storage tanks, thereby dynamically adjusting the proportions to avoid residual organic residues or excessive loss of iron ions. Ultimately, this significantly improves the stability and batch-to-batch repeatability of iron recovery rate, while achieving fully automated and precise operation and eliminating human intervention errors. Attached Figure Description

[0013] Figure 1 This is an isometric view of the present invention; Figure 2 This is a diagram of the internal structure of the present invention; Figure 3 This is a structural diagram of the storage tank of this utility model; Figure 4 This is a top view of the present invention.

[0014] Legend: 1. Reaction vessel; 2. Controller; 3. Storage tank; 4. Detector; 5. Stirring assembly; 501. Servo motor; 502. Rotating rod; 503. Stirring rod; 6. First support leg; 7. Connecting pipe; 8. Flow sensor; 9. First solenoid valve; 10. Heating assembly; 11. Guide pipe; 12. Drain pipe; 13. Second solenoid valve; 14. Gas outlet pipe; 15. Second support leg. Detailed Implementation

[0015] To make the technical means, creative features, and achieved objectives and effects of this utility model easier to understand, the present utility model is further described below with reference to specific embodiments and accompanying drawings. However, the following embodiments are merely preferred embodiments of this utility model and not all of them. Other embodiments obtained by those skilled in the art based on the embodiments described in the implementation plan without creative effort are all within the protection scope of this utility model.

[0016] The specific embodiments of this utility model are described below with reference to the accompanying drawings. Specific Implementation Example 1: Reference Figure 1-4 An automatic digestion device for pretreatment of sodium ferrochlorophyllin samples includes a reaction vessel 1 and a storage tank 3. The top surface of the reaction vessel 1 is provided with a first support leg 6, the end of which is connected to the bottom surface of the storage tank 3. The reaction vessel 1, as the core reaction container, is made of acid-resistant and high-temperature-resistant material and is used to hold the sodium ferrochlorophyllin sample and digesting agent. Three sets of storage tanks 3 are dedicated to storing concentrated nitric acid (main oxidant), 30% hydrogen peroxide (auxiliary oxidant), and pure water (diluent / rinsing agent), respectively. A connecting pipe 7 is connected to the bottom surface of each tank, and the three sets of storage tanks 3 are fixed to the first support leg on the top surface of the reaction vessel 1. At the six ends, a compact layout and independent flow path supply are achieved through a circumferential array, supporting dynamic proportioning and replenishment, avoiding cross-contamination and ensuring that raw materials are injected in a gradient as needed. The first support leg 6 serves to mechanically support the array of storage tanks 3. A controller 2 is installed on the surface of the reaction tank 1. The controller 2 is electrically connected to the detector 4 and the first solenoid valve 9. The controller 2 is an industrial-grade PLC integrating an AI chip and a touch screen. It is fixed to the middle of the reaction tank 1 and electrically connected to the detector 4, the first solenoid valve 9, the flow sensor 8, the servo motor 501, the heating component 10, and the second solenoid valve 9. The electrically controlled valve 13 calculates the initial ratio after sample quality input, collects multiple parameters from detector 4 every 30 seconds, uses AI algorithms to judge digestion deviation in real time and outputs supplementation instructions, controls temperature or stirring according to the program, and stores and exports data logs and reports, realizing fully closed-loop intelligent control and compliance traceability. Detectors 4 are installed on the surface of reaction vessel 1. Three sets of detectors 4 are arranged in a circular array between storage tank 3 and connecting pipe 7. The bottom probes of detectors 4 extend into the interior of storage tank 3 to collect data. These detectors are absorbance detector 4, conductivity detector 4, and pH detector 4. The absorbance detector 4 has a miniature spectrometer that measures the phytophyte characteristic peak in real time and calculates the organic degradation rate, which can reflect the progress of complex pyrolysis and determine whether the organic matter has been completely decomposed. The conductivity detector 4 monitors the rate of change in solution conductivity, which can quantify the release of iron ions and determine whether iron ions have been fully released. The pH detector 4 tracks the acidity consumption curve, measures acidity and alkalinity changes, and determines the oxidant balance and reaction endpoint. Multidimensional real-time data is provided by the three detectors 4 and input into controller 2 to trigger dynamic adjustments.

[0018] The reaction vessel 1 is equipped with a stirring assembly 5, which includes a servo motor 501, a rotating rod 502, and a stirring rod 503. The rotating rod 502 is vertically fixed to the output end of the servo motor 501, and the stirring rod 503 is horizontally fixed to the rotating rod 502. The servo motor 501 is fixed to the outside of the bottom of the reaction vessel 1, and its output shaft is sealed to the rotating rod 502. The stirring rod 503 has multiple layers on its surface. The servo motor 501 drives the rotating rod 502 to rotate, thereby driving the stirring rod 503 to stir, promoting uniform mass transfer, preventing local overheating and sedimentation. To improve reaction efficiency and consistency, a connecting pipe 7 is installed on the bottom of storage tank 3, with a flow sensor 8 on the connecting pipe 7 and a first electrically controlled valve 9. The bottom end of the connecting pipe 7 is directly connected to the inlet of the cover of reaction tank 1. Its function is to safely transport raw materials, prevent backflow and leakage, and support micro-precision injection. The flow sensor 8 is a pipeline flow meter that measures the actual injection volume in real time. The feedback controller 2 realizes closed-loop calibration to ensure the accuracy of the ratio. The first electrically controlled valve 9 is a high-speed solenoid valve that receives signals from the controller 2 to realize opening and closing, and controls the flow of three groups of raw materials as needed. The flow rate is controlled by a flow sensor 8, which precisely executes commands. A heating assembly 10 is installed inside the reaction vessel 1, electrically connected to the controller 2. The heating wire in the heating assembly 10 is located in and surrounds the side wall of the reaction vessel 1. A heat-insulating coating is provided on the outer surface of the side wall of the reaction vessel 1. A drain pipe 12 is provided on the bottom surface of the reaction vessel 1, and a guide pipe 11 is provided on the top surface. A second electrically controlled valve 13 is provided on the surface of both the guide pipe 11 and the drain pipe 12. An exhaust pipe 14 is provided on the surface of the reaction vessel 1, and a second support leg is provided on the bottom surface of the reaction vessel 1. 15. The heating component 10 realizes segmented program heating, which accelerates oxidation decomposition and removes residual acid. The guide pipe 11 is the inlet of the initial sample. The drain pipe 12 automatically discharges the solution to the collection bottle after digestion and supports sampling and analysis after volume adjustment. The second electric control valve 13 is uniformly managed by the controller 2, which controls the inlet and outlet of the material in a sealed manner to prevent leakage and pollution and ensure the process is closed and safe. The exhaust pipe 14 is connected to the tail gas condensation and absorption tower to export acid mist or waste gas in real time, achieving zero emission and environmental protection. The second support leg 15 is used to stabilize the whole device, prevent tipping, and facilitate installation on the laboratory table. Specific Implementation Example 2: An automated digestion device for pretreatment of sodium ferrochlorophyllin samples, based on the basic structure in Specific Embodiment 1, further discloses the following: The operator first places the weighed sodium ferrochlorophyllin sample into the reaction vessel 1 through the guide tube 11 and seals it. Then, the operator inputs the sample mass on the touchscreen of the controller 2. The controller 2 automatically calculates the initial ratio and instructs three sets of first electrically controlled valves 9 to open simultaneously. Flow sensors 8 measure in real time the injection of the main oxidant into the nitric acid storage tank 3, the injection of the auxiliary oxidant into the hydrogen peroxide storage tank 3, and the preparation of the pure water storage tank 3 for dilution. The heating component 10 starts a segmented program to heat to the pre-digestion stage. Simultaneously, the servo motor 501 drives the rotating rod 502 and the stirring rod 503 to stir evenly. At fixed intervals, three detectors 4 synchronously collect data, and the absorbance detector 4 measures... The organic degradation rate is calculated using phytomorph characteristic peaks; conductivity detector 4 monitors the rate of change in conductivity to quantify iron ion release; pH detector 4 tracks the acidity consumption curve to determine oxidation balance; controller 2, through algorithm analysis, detects progress deviations (such as insufficient organic degradation or risk of iron loss) and immediately instructs the corresponding first electronic control valve 9 to open with a pulse; flow sensor 8 provides closed-loop feedback to accurately replenish nitric acid, hydrogen peroxide, or pure water until parameters return to normal; three sets of storage tanks 3 independently cycle and dynamically adjust the ratio; the reaction process steadily progresses to the main digestion and acid removal stage; exhaust pipe 14 discharges waste gas to the tail gas absorption system throughout the process; after automatic stop at the digestion endpoint, the second electronic control valve 13 opens the drain pipe 12 to discharge the solution to the collection bottle to support subsequent volumetric analysis; the entire process data log is stored and reports can be exported.

[0020] In summary: 1. The system employs three sets of storage tanks 3, three detectors 4, a flow sensor 8, and a first electrically controlled valve 9. The three detectors 4 enable real-time multi-point monitoring of the digestion solution, including parameters such as absorbance, conductivity, and pH. The controller 2 collects multi-parameter signals from the three detectors 4 in real time. When the detectors 4 detect a deviation in the digestion progress, the controller 2 immediately instructs the corresponding first electrically controlled valve 9 to open or close. Based on feedback from the flow sensor 8, the controller accurately measures the amount of nitric acid, hydrogen peroxide, and pure water added to the three sets of storage tanks 3, thereby dynamically adjusting the proportions to avoid residual organic residues or excessive loss of iron ions. This significantly improves the stability and batch-to-batch repeatability of iron recovery rate, while achieving fully automated and precise operation and eliminating human intervention errors.

[0021] In this invention, unless otherwise explicitly specified and limited, "above" or "below" the second feature can include direct contact between the first and second features, or contact between the first and second features through another feature between them. Furthermore, "above," "over," and "on top" of the second feature includes the first feature directly above or diagonally above the second feature, or simply indicates that the first feature is at a higher horizontal level than the second feature. "Below," "below," and "under" the second feature includes the first feature directly below or diagonally below the second feature, or simply indicates that the first feature is at a lower horizontal level than the second feature.

[0022] The foregoing has shown and described the basic principles, main features, and advantages of this utility model. Those skilled in the art should understand that this utility model is not limited to the above embodiments. The embodiments and descriptions in the specification are merely preferred examples and are not intended to limit the utility model. Various changes and modifications can be made to this utility model without departing from its spirit and scope, and all such changes and modifications fall within the scope of the claimed utility model. The scope of protection of this utility model is defined by the appended claims and their equivalents.

Claims

1. An automated digestion device for pretreatment of sodium ferrochlorophyllate samples, comprising a reaction vessel (1) and a storage tank (3), characterized in that: The surface of the reaction vessel (1) is provided with a detector (4), the probe end of the detector (4) extends into the interior of the storage tank (3), the interior of the reaction vessel (1) is provided with a stirring assembly (5), the bottom surface of the storage tank (3) is provided with a connecting pipe (7), the connecting pipe (7) is provided with a flow sensor (8) and a first electrically controlled valve (9), the interior of the reaction vessel (1) is provided with a heating assembly (10), and the bottom surface of the reaction vessel (1) is provided with a drain pipe (12).

2. The automatic digestion device for pretreatment of sodium ferrochlorophyllate samples according to claim 1, characterized in that: The stirring assembly (5) includes a servo motor (501), a rotating rod (502) and a stirring rod (503). The output end of the servo motor (501) is vertically fixed with the rotating rod (502), and the stirring rod (503) is horizontally fixed on the rotating rod (502).

3. The automatic digestion device for pretreatment of sodium ferrochlorophyllate samples according to claim 2, characterized in that: The surface of the reaction vessel (1) is provided with a controller (2), which is electrically connected to the detector (4), the servo motor (501), the heating component (10) and the first electrically controlled valve (9).

4. The automatic digestion device for pretreatment of sodium ferrochlorophyllate samples according to claim 1, characterized in that: The top surface of the reaction vessel (1) is provided with a first support leg (6), and the end of the first support leg (6) is connected to the bottom surface of the storage tank (3).

5. The automatic digestion device for pretreatment of sodium ferrochlorophyllate samples according to claim 1, characterized in that: The top surface of the reaction vessel (1) is provided with a guide pipe (11), and the surfaces of the guide pipe (11) and the drain pipe (12) are both provided with a second electrically controlled valve (13).

6. The automatic digestion device for pretreatment of sodium ferrochlorophyllate samples according to claim 1, characterized in that: The storage tank (3) and the connecting pipe (7) are arranged in three sets in a circular array, and the detector (4) is arranged in three sets in a circular array.

7. The automatic digestion device for pretreatment of sodium ferrochlorophyllate samples according to claim 1, characterized in that: The surface of the reaction vessel (1) is provided with an exhaust pipe (14), and the bottom surface of the reaction vessel (1) is provided with a second support leg (15).

8. The automatic digestion device for pretreatment of sodium ferrochlorophyllate samples according to claim 1, characterized in that: The heating wire in the heating assembly (10) is located in the side wall of the reaction vessel (1) and is arranged around it. The side wall of the reaction vessel (1) is provided with a heat insulation coating on the outer surface.

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