A multifunctional fully automatic iodine sample injection device and analyzer

Abstract

The present invention provides a fully automatic sampling device for a variety of iodine samples, including a base, a three-axis sampling module, a multifunctional sampling needle, an integrated digestion constant temperature module, a reagent sampling module, and a pumping circulation module. The present invention also provides a multifunctional fully automatic iodine element analyzer including the fully automatic sampling device, a cleaning module, and a multi-band photoelectric detection module. The present invention uses three motion modules and a multifunctional sampling needle to complete the functions of reagent addition, mixing, sample transfer measurement, etc. in the non-through-hole positions in the entire experiment. At the same time, the multifunctional sampling needle adopts different drop designs, combined with the technology of multiplexing pipelines and the pipeline rinsing process, to achieve the multiplexing of the sampling needle pipeline, and the use of two reagent needles can achieve the cross-contamination-free addition of multiple reagents. The present invention combines the above-mentioned fully automatic sampling device with the selection of different light sources and automation processes in the photoelectric detection module to obtain a fully automatic analyzer that detects a variety of different iodine samples.

Description

Technical Field

[0001] The invention belongs to the field of analytical instruments, and particularly relates to a full-automatic intelligent iodine sample injection device and an analyzer thereof. Background Art

[0002] Iodine, an essential raw material for the human body, is known as the "element of intelligence." The total iodine content in a healthy adult is approximately 30 mg (20-50 mg), of which 70%-80% is found in the thyroid gland. People primarily obtain iodine from drinking water, food, vegetables, and the surrounding environment. Both iodine deficiency and excess can cause thyroid-related diseases, making the determination of iodine content crucial in daily life.

[0003] We possess comprehensive testing methods for iodine intake in fields such as environmental protection, food, and disease control and hygiene. Different methods and standards are employed by various industries based on their testing needs. In the field of disease control and hygiene, we primarily analyze iodine content in drinking water and human urine using traditional manual testing and analysis in accordance with standards such as "GB-T 5750.5-2006 Standard Test Method for Drinking Water - Inorganic Non-metallic Indices" and "WST 107.1-2016 Determination of Iodine in Urine - Part 1: Arsenic-Cerium Catalytic Spectrophotometry." In the food industry, iodized salt is primarily tested in accordance with "GBT 13025.7-2012 General Test Methods for Salt Production Industry - Determination of Iodine."

[0004] Traditional iodine analysis in solutions is primarily based on the principle of arsenic-cerium catalytic spectrophotometry, which involves a slow redox reaction between arsenous acid and ceric sulfate under acidic conditions. Iodide ions catalyze the reduction of yellow Ce₄+ to colorless Ce₃+. The higher the iodine content, the faster the reaction, resulting in less residual Ce₄+. By controlling the reaction temperature and time, the absorbance of the residual Ce₄+ in the system is colorimetrically determined. The iodine content is calculated using the linear relationship between the iodine mass concentration and the logarithm of the measured absorbance.

[0005] H3AsO3+2Ce 4+ +H2O→H3AsO4+2Ce 3+ +2H +

[0006] For urinary iodine, the urine sample must be digested with ammonium persulfate at 100°C to release free iodine, which can then be measured. For details, see GB-T 5750.5-2006 Standard Test Methods for Drinking Water - Inorganic Non-metallic Indices and WST 107.1-2016 Determination of Iodine in Urine - Part 1: Arsenic-Cerium Catalytic Spectrophotometry.

[0007] However, for iodine in solid substances (such as iodine in table salt), the measurement principle is different from the above principle: the iodized salt is dissolved in distilled water in advance, and then in an acidic medium, the iodate ions in the sample oxidize potassium iodide to precipitate elemental iodine, which is then titrated with sodium thiosulfate standard titrant to determine the iodine content. The specific reaction formula is as follows:

[0008] IO3 - +5I - +6H - →3I2+3H2O 2S2O3 2- +I2→2I - +S4O5 2-

[0009] Both of the above-mentioned two different methods require the experimenter to operate at a fixed time and in a fixed quantity, using timers, digesters, constant temperature water baths, spectrophotometers, etc. to perform digestion, insulation, timing, and spectrophotometric detection. The operation process is complicated, and the experiment has extremely high requirements for temperature and time. Therefore, the data stability and accuracy of traditional manual operations are difficult to control.

[0010] In recent years, with the improvement of people's health awareness, the increase in testing needs, and the country's continuous investment in the field of disease control and health, the market demand for automated iodine measurement has gradually matured, and corresponding automated testing equipment has appeared on the market. One type of this type of equipment follows the design structure of the full-automatic biochemical analyzer technology route, which has disadvantages such as large size, complex structure, and high manufacturing and maintenance costs. The other type uses a design method that uses mechanical grippers to simulate manual operations, with high system complexity, high construction and maintenance costs, and low system reliability.

[0011] Chinese invention patent application 201810137209.0, "A Fully Automatic Intelligent Urine Iodine Analyzer and Its Operating Method," discloses a fully automatic intelligent urine iodine analyzer comprising a housing, a sample carrier mechanism, a reagent dosing device, an optical path detection system, a comprehensive sample handling mechanism, a waste tank, and an electronic control system. The analyzer utilizes a quantitative colorimetric method, controlling the rotation of a reagent tray to achieve point-to-point operation of various reagents. A sample dosing and stirring device is used to mix the test reagents, preventing cross-contamination and improving mixing efficiency. A dual-needle dosing arm enables the addition of developer and oxidant, shortening test time and conserving internal and external space. The analyzer also features automatic result interpretation and report printing, enhancing the automation of urine iodine testing. According to the current standard "WST 107.1-2016: Determination of Iodine in Urine - Part 1: Arsenic-Cerium Catalytic Spectrophotometry," urine iodine testing requires high-temperature sample digestion, followed by constant-temperature testing after reagent addition. However, this invention lacks a high-temperature digestion device or any temperature control device, making it impossible to achieve fully automated urine iodine measurement. At the same time, the liquid transfer and addition mechanical structure of the invention adopts a turntable mechanism (including 210, 220, 231, 225, etc.), a lifting arm liquid addition system (including 311, 312, 314, 315, 319, 320, etc.), and a vertical displacement mechanism (including 516, 517, 518, 529, 541, etc.). The motion logic includes a turntable (instruction manual 0138), horizontal displacement (instruction manual 0139), vertical displacement (instruction manual 0139), axis rotation (instruction manual 0148), and axis lifting (instruction manual 149). The entire solution has many components and complex logic. In addition, the invention lacks a pollution-free cleaning device for the inner and outer walls of the injection needle. In order to prevent cross-contamination during the measurement process, additional disposable consumables (pipettes) are required. Some pipette tips need to be manually installed and replaced (instruction manual 0146). The operation is cumbersome, the operation requires consumables support, the cost is increased, and the pipette tips that come into contact with the test solution are rich in arsenic, causing secondary environmental pollution.

[0012] Chinese Utility Model Patent No. 201721854009.4, "A Urine Iodine Analyzer," discloses a urine iodine analyzer comprising a housing, a mixing mechanism, a detection mechanism, and a control unit. A first slot is provided on one side wall of the housing, into which a cuvette is removably received, and coaxial detection holes are provided on opposite side walls of the first slot. The mixing mechanism is used to uniformly mix the urine to be tested and the chemical reagent in the cuvette. The detection mechanism is disposed within the housing and is used to detect and analyze the urine to be tested in the cuvette. Similarly, this device lacks an automatic digestion device, making it incapable of fully automated urine iodine measurement and unsuitable for analyzing water or salt iodine.

[0013] Chinese invention patent application No. 202010533643.8, "A Vision-Based Automatic Measurement Device and Method for Iodine Content in Table Salt," discloses a vision-based automatic measurement device for iodine content in table salt. The device comprises a micro-dosing pump module, a test liquid container, a magnetic stirrer, an annular light source, an industrial camera, an industrial lens, a display screen, a controller module, a light-shielding housing, and a hose assembly. The micro-dosing pump module and controller module are located on either side of the light-shielding housing, respectively. The test liquid container, annular light source, and industrial lens are located within the light-shielding housing. The magnetic stirrer is located below the light-shielding housing. The industrial camera is located within the controller module, and the display screen is located on the side of the controller module. However, this device is based on Method 3 (Redox Titration) in GBT 13025.7-2012, "General Test Methods for Salt Production Industry - Determination of Iodine," and therefore can only be used to test salt iodine, not water or urine iodine.

[0014] Chinese Utility Model Patent No. 202021205027.1, "A Novel Iodine Analyzer with Automatic Digestion," discloses an iodine analyzer with automatic digestion, characterized by comprising a base and a porous heating furnace mounted on the base; the porous heating furnace having a plurality of heating holes for receiving sample tubes; a bottom opening of each heating hole communicating with a cavity within the porous heating furnace; a cooling water inlet and a cooling water outlet provided within the cavity; an overflow hole formed in the upper portion of the porous heating furnace; and a drain port II connected to the bottom of the base. Although the device incorporates both a digestion device and a constant temperature water bath, automating iodine analysis and simplifying automated iodine analysis detection, the invention essentially improves the digestion and constant temperature water bath components of the iodine analyzer. It does not improve components such as the sample loading and optical detection components, nor does it specify whether it can be used to analyze samples such as salt iodine. Most importantly, because the analytical reagent arsenite is highly toxic and contaminating, the piping leading to the sample tube lacks one-way sealing or overflow or backflow prevention features (for example, no dosing pump), posing a risk of environmental contamination. Furthermore, the invention merely improves the aforementioned components and does not disclose a specific iodine analysis device.

[0015] As a relatively close prior art, Chinese invention patent application 202010326714.7, Fully Automatic Urine Iodine and Water Iodine Analyzer and Analysis Method (see Patent No. 09), discloses a fully automatic urine iodine and water iodine analyzer and analysis method, wherein the fully automatic urine iodine and water iodine analyzer includes an analyzer body, which includes a workbench and a three-dimensional motion platform arranged on the workbench, a graphite digestion device, a water bath container, a sample rack, a stirrer, a cleaning device and a detection device. The most important innovation of this invention is the use of a three-dimensional motion platform with a manipulator to achieve the grasping of sample tubes in the X / Y / Z axis directions. In addition, three injection capillaries are provided on the manipulator to add ammonium sulfate solution, arsenous acid solution and ammonium cerium sulfate solution into the sample tube through the three injection capillaries; and an injection needle can also be provided on the manipulator to absorb the sample in the sample tube through the injection needle and inject the sample into the detection device. However, the defects of this invention are as follows: (1) When the manipulator grabs the sample tube, there is a possibility of failure in grabbing and transferring, and additional complex components are required (such as positioning components, manipulator opening and contracting components and their control components); (2) In order to facilitate sample mixing, a vortex mixing oscillator is added, which not only makes the structure more complicated, but also pauses the processing of the next sample because the current sample is shaken and mixed, affecting the analysis speed of multiple samples; (3) This patent uses a hot water circulation device connected to the water bath container and a circulation pump with a heating function. This circulation pump requires regular maintenance and is difficult to maintain; (4) The photoelectric detection module is a traditional silicon photodiode or photomultiplier tube or CCD detector (see paragraph 058), which has a low light source irradiation utilization rate, large heat radiation loss, and high energy consumption. At the same time, this invention involves a single light source and cannot cover the detection needs of different samples and different concentrations. (5) This invention designs a sample rack, a graphite digestion area, etc., and an external hot water circulation device, which has a low space reuse rate, a large equipment footprint, and low digestion and measurement efficiency.

[0016] As the closest existing technology, Chinese utility model patent 202023023930.9, a new type of fully automatic salt iodine analyzer (see Patent No. 07) discloses a salt iodine analyzer, including a workbench, a three-dimensional motion mechanism, a high-precision liquid adding device, a peristaltic pump I, a cooling device, a continuous detection photometer, a sample rack, a sample test tube, an external container bottle, a liquid adding and stirring sampling needle, and a waste liquid collection bottle. The principle of the invention is that the high-precision liquid adding device selects a fixed volume of pure water, one of reagent A and reagent B, and uses a high-precision metering pump to deliver it to the liquid adding and stirring sampling needle through a pipeline. Under the action of the three-dimensional motion mechanism, the liquid adding and stirring sampling needle sends different liquids into different sample test tubes for reaction; in order to quickly achieve sample dissolution and reaction stirring, when the liquid is sent into the sample test tube, the peristaltic pump I is started in reverse. At this time, the peristaltic pump I and the liquid adding and stirring sampling needle form a reverse bubble stirring device, which sucks in reverse air from the joint, passes through several pipelines, and the continuous detection photometer from the liquid adding and stirring Liquid is blown out of the sampling needle and into the liquid in the sample tube, achieving a stirring function. Once the sample solution in the sample tube has reacted, the three-dimensional motion mechanism carries the liquid-adding and stirring sampling needle to each sample tube in turn to sample. During this process, peristaltic pump I is activated in the forward direction. At this time, peristaltic pump I, the continuous detection photometer, and the liquid-adding and stirring sampling needle form a flow cell continuous detection device. The liquid-adding and stirring sampling needle continuously feeds the sample solution from each sample tube through a pipeline to the continuous detection photometer for testing. The test waste liquid is then discharged through the waste outlet into a waste liquid collection bottle for collection. After testing of a sample solution is completed, the three-dimensional motion mechanism carries the liquid-adding and stirring sampling needle to a cleaning sink to draw clean water. The needle, pipeline, peristaltic pump I, and continuous detection photometer are then cleaned before the next sample is sampled and tested. Although this invention proposes the concept of reversing bubbles to stir the sample solution, the sampling needle simultaneously fills the sample to be tested and the reagent, requiring separate cleaning of the sampling needle each time a different sample or reagent is added. At the same time, in order to achieve the addition of three reagents, it is necessary to set up three three-way valves, resulting in a complex structure and difficult maintenance. In addition, the sample to be tested enters the continuous detection photometer 5 through the peristaltic pump I4 and then enters the waste liquid collection bottle. As a result, when the sample passes through the transfer pump, the detached substances and precipitates that may be generated during the peristaltic process of the pump tube affect the test results. Most importantly, the device lacks a digestion device and can only be used to test salt iodine, and cannot analyze water iodine and urine iodine.

[0017] In summary, the existing technology is still suitable for inventing a single analyzer for measuring water iodine, urine iodine, and salt iodine according to the standards of "GB-T 5750.5-2006 Standard Test Method for Drinking Water - Inorganic Non-metallic Index", "WST 107.1-2016 Determination of Iodine in Urine Part 1: Arsenic-Cerium Catalytic Spectrophotometry", and "GBT13025.7-2012 Salt Industry General Test Method Determination of Iodine". There is a lack of an analyzer that can measure three types of iodine.

[0018] Therefore, there is a need for an analyzer capable of measuring three types of iodine. Compared to previous iodine analyzers, this device should firstly be able to apply three standard detection principles. Secondly, it should be able to quickly digest urine samples with high impurities and automatically heat and maintain a constant temperature for water samples. Finally, the analyzer should also have advantages such as simple and convenient sample addition, no contamination of reagent lines, and easy cleaning of the lines. Summary of the Invention

[0019] The first inventive principle of the present invention is to provide a fully automatic iodine analyzer that is simultaneously applicable to the standards of "GB-T 5750.5-2006 Standard Test Method for Drinking Water - Inorganic Non-metallic Indices", "WST 107.1-2016 Determination of Iodine in Urine Part 1: Arsenic-Cerium Catalytic Spectrophotometry", and "GBT 13025.7-2012 General Test Methods for Salt Production Industry - Determination of Iodine". To this end, based on the existing technology, a three-axis injection module, a multi-function injection needle, an integrated digestion constant temperature module integrating metal bath and water bath functions, a cooling device, and a reagent injection module have been redesigned, so that different samples such as water iodine, urine iodine, and salt iodine can be detected.

[0020] Specifically,

[0021] (1) The three-axis injection module, combined with the multifunctional injection needle, can replace the three-dimensional mobile manipulator or device to grasp the sample tube, effectively reducing the mechanical risk of grasping and transfer failure, and significantly reducing production costs;

[0022] (2) The multifunctional injection needle with different drop designs can prevent sample contamination of the reagent line or cross contamination when the sample needle and reagent needle are used at the same time;

[0023] (3) The bubbles blown by the reagent needle are used to achieve liquid mixing and stirring, reducing the complex structure brought by the turbine oscillation mixing device;

[0024] (4) An integrated digestion and constant temperature module that integrates the functions of a metal bath and a water bath, with a diaphragm pump as the water supply pump and drain pump, can quickly replenish or drain water without requiring regular maintenance. Under computer control, this module can select digestion and / or heat preservation according to the sample type, thereby enabling the analyzer to universally analyze water iodine, urine iodine, and salt iodine.

[0025] (5) The cooling module can achieve rapid cooling of the temperature after digestion, greatly reducing cooling water and cooling time, improving system measurement efficiency, and reducing waste liquid discharge;

[0026] (6) The digestion constant temperature module is equipped with an air duct running through both ends of the base, and fans are installed at the positions near both sides of the base. When the fan is turned on, a forced air cooling zone is formed to achieve sample condensation and reflux during the digestion process and reduce sample volatilization. The actual verification shows that the volatilization rate of the digested sample is <1%, which is a significant improvement compared to the 25% to 30% volatilization rate of traditional digestion. As a result, the sample after digestion can be automatically analyzed without manual replenishment of pure water. After the digestion is completed, when the system needs to be kept at a constant temperature, the fan will be automatically turned off. There is no relative flow of gas in the original air cooling zone, which is transformed into a constant temperature zone, isolating the water bath from the outside of the instrument, further improving the constant temperature effect.

[0027] (7) The reagent injection module adopts a multi-channel time-sharing multiplexing design, combined with an automated controller and related programs. It can not only realize the reagent addition function, but also realize the addition of multiple different reagents through the coordination of switching valves, thereby completing the analysis of different iodine samples.

[0028] In summary, the fully automatic iodine analyzer with the above components, combined with the existing photoelectric detection module and waste liquid cleaning and recovery module, can obtain an analyzer that can universally analyze water iodine, urine iodine, and salt iodine.

[0029] The second inventive principle of the present invention is based on the above principle, introducing a low-consumption and high-efficiency multi-band photoelectric detection module and an integrated multifunctional needle washing waste liquid pool to improve the efficiency of the whole machine's automated analysis. Specifically,

[0030] (1) The multi-band photoelectric detection module adopts a low-power LED and photocell detection solution. Compared with conventional photoelectric detection modules, it effectively improves the utilization rate of light source radiation, making the energy consumption of the entire LED power supply control system extremely low. It can not only reduce the thermal radiation of the photoelectric detection module and the drift of the entire photoelectric detection system, but also enable the system to quickly reach thermal stability and improve the system's ease of use and reliability.

[0031] (2) The integrated multifunctional needle washing waste liquid pool can not only achieve pollution-free cleaning of sample needles, but also realize automatic overflow discharge of waste liquid. It can also collect high-temperature wastewater generated during the water cooling process of the integrated digestion constant temperature module, as well as waste liquid during the detection process and waste liquid during the cleaning of reagent pipelines;

[0032] Therefore, the first object of the present invention is to provide a fully automatic sampling device for multiple iodine samples, which can fully automatically sample different samples such as water iodine, urine iodine, and salt iodine, including a base, a three-axis sampling module, a multifunctional sampling needle, an integrated digestion constant temperature module, a reagent sampling module, and a pumping circulation module, characterized in that:

[0033] (1) The base is the base of the analyzer, with a sample table on the upper surface for placing samples, and an integrated digestion constant temperature module, photoelectric detection module, needle washing module, reagent injection module, and pumping circulation module inside;

[0034] (2) A three-axis injection module located above the base, including three modules in the X (horizontal) direction, the Y (front and back) direction, and the Z (up and down) direction. The end of the Z module is fixedly connected to the multifunctional injection needle, and the three-axis injection module can realize the programmable displacement of the multifunctional injection needle in the up, down, left, right, front and back directions;

[0035] (3) The multifunctional injection needle is composed of a first reagent needle, a sample needle, and a second reagent needle from left to right. The three needles are integrally formed using a bonding / welding technique, wherein the end of the central sample needle protrudes from the ends of the first and second reagent needles on both sides, so that when the central sample needle is immersed in the liquid, the first and second reagent needles on both sides are located above the liquid surface, thereby preventing the sample from contaminating the reagent line and preventing cross contamination between the reagent lines;

[0036] (4) The main body of the integrated digestion constant temperature module is located inside the base, including the sample tube, heating body, temperature sensor, temperature control module, water bath, and air cooling channel;

[0037] The sample tube is located inside the base of the multifunctional injection needle, which is vertically facing downward. The lower part is located in the heating body, and the upper part is located in the air cooling channel running through both ends of the base. A temperature sensor is installed inside the heating body, and a water bath is installed outside to provide a constant temperature environment for the sample tube. The bottom of the water bath is equipped with multiple water supply and drainage interfaces. In addition, a temperature sensor is installed outside the base.

[0038] (5) The reagent injection module includes a first reagent container, a second reagent container and / or a third reagent container, and a second liquid adding pump and a first liquid adding pump for driving the first, second and / or third reagent into the first or second reagent needle, and a transfer pump for driving the sample or air into the sample needle;

[0039] (6) The pumping circulation module includes a water supply pump, a drainage pump, and a circulation pump, wherein the water supply pump and the drainage pump are arranged in parallel alternately, that is, the water outlet of the water supply pump is connected to the water inlet of the drainage pump and connected to a water supply and drainage interface of the water bath, and the water inlet of the water supply pump is connected to the water outlet of the drainage pump and connected to the water tank outside the equipment. By opening the water supply pump and the drainage pump separately, the water bath can be supplied with water and drained; the water inlet and water outlet of the circulation pump are respectively connected to different water supply and drainage interfaces of the water bath, so that the water in the water bath can circulate as needed to maintain a constant temperature environment.

[0040] In one embodiment, when the sample needle adds the sample to be tested to the sample tube, and / or the first or second reagent needle located above the liquid surface adds the reagent to the sample tube, the sample needle located below the liquid surface is driven by a transfer pump to allow gas to enter the sample tube through the sample needle, thereby achieving gas mixing and stirring, and achieving contactless addition of the first and second reagents, thereby reducing contact contamination;

[0041] In another embodiment, the analyzer further comprises a multifunctional needle washing waste liquid pool, so that the multifunctional injection needle is transferred to the waste liquid pool for cleaning after adding the sample.

[0042] In one embodiment, fans are provided at both ends of the air-cooling channel of the digestion constant temperature module, so that when the fans are turned on, an air-cooling zone is formed to achieve sample condensation and reflux during the digestion process and reduce sample digestion and volatilization, while when the fans are turned off, a constant temperature zone is formed.

[0043] In one embodiment, a heat-insulating plate is provided between the air-cooling channel and the water bath, and a heat-insulating jacket is provided on the outer surface of the water bath.

[0044] In one embodiment, the heating body is made of a heat-conducting material and has a heating rod disposed therein.

[0045] In other embodiments, the second reagent container and the third reagent container are designed in parallel, and a switching valve is provided at the parallel intersection, so that the second adding pump drives the second reagent or the third reagent into the first reagent needle, and the first adding pump drives the first reagent into the second reagent needle, thereby achieving the addition of different reagents for different iodine samples.

[0046] In any of the above embodiments, the fully automatic sampling device, in conjunction with the automation controller and related programs, realizes the reuse of sampling needle pipelines and the analysis of different water iodine, urine iodine, and salt iodine samples by controlling the start-up of the digestion constant temperature module and the order of adding different reagents.

[0047] In a specific embodiment, a cooling device can be connected in series in the flow path of the circulation pump of the pumping circulation module. When detecting urine iodine samples, the automatic controller will turn on the cooling module when the water bath is kept at a constant temperature after digestion, which can quickly cool the high-temperature water to a constant temperature, thereby improving system efficiency and reducing process water use.

[0048] The second object of the present invention is to provide a multifunctional fully automatic iodine element analyzer, which includes the fully automatic sampling device described in any of the above schemes, as well as a cleaning module and a multi-band photoelectric detection module.

[0049] In one embodiment, the cleaning module includes an integrated multifunctional needle washing waste liquid pool and a liquid transfer pipeline, wherein the multifunctional needle washing waste liquid pool includes a pure water tank, a needle washing pump, a needle washing pool inlet, a needle washing pool, an overflow port, a first waste liquid chamber, a second waste liquid chamber, a first waste liquid port, and a second waste liquid port in order of connection, wherein the needle washing pool is connected to the first waste liquid chamber through the overflow port at the top, the first waste liquid chamber is connected to the bottom of the second waste liquid chamber through the connecting port at the bottom, the first waste liquid port is located at the upper part of the second waste liquid chamber, and the second waste liquid port is located at the lower part of the second waste liquid chamber.

[0050] In another embodiment, the multi-band photoelectric detection module is provided with a module communication interface, a rotating motor, a rotating light source board, an LED lamp bead, a first focusing lens, a circulation colorimetric cell, a second focusing lens, and a photoelectric detection board in sequence according to the direction of travel of the light path, wherein the first and second focusing lenses are provided at both ends of the circulation colorimetric cell, and the upper end is provided with a passage for receiving the sample solution to be tested from the sample needle, and a passage connected to the first waste liquid port.

[0051] In a preferred embodiment, the sample solution to be tested in the sample tube is drawn into the circulation colorimetric cell through a transfer pump provided on the passage connecting the circulation colorimetric cell and the first waste liquid port through a sample needle. The rotating motor rotates the LED lamp beads of a preset wavelength to align with the light path by rotating the light source plate. The light emitted by the light source passes through the first focusing lens, the circulation colorimetric cell, and the second focusing lens respectively until it is focused on the photocell detection board. The photocell detection board converts the detected light signal into an electrical signal, which is transmitted to the main control board and the computer by the module communication interface. In a more preferred embodiment, the solution after passing through the circulation colorimetric cell enters the first waste liquid interface of the multifunctional needle washing waste liquid pool through a transfer pump. The waste liquid flows downward due to gravity and is discharged from the device through the second waste liquid interface.

[0052] In any of the above embodiments, after the measurement is completed, the needle washing pump is turned on, and the pure water in the pure water tank is injected into the needle washing pool through the needle washing pool inlet, and the three-axis injection module is moved so that the multifunctional injection needle is inserted into the needle washing pool to complete the cleaning; the sewage flows into the first waste liquid chamber through the overflow port, and is discharged from the second waste liquid interface through the connecting port at the bottom.

[0053] The third object of the present invention is to provide a fully automatic sample introduction device, a cleaning module and / or a multi-band photoelectric detection module comprising any of the above schemes, for use in a fully automatic analyzer for preparing a variety of iodine samples of different specifications.

[0054] In one embodiment, the fully automatic sample injection device, cleaning module and / or multi-band photoelectric detection module are all modularly designed and can replace the existing iodine analyzer to obtain iodine analyzers of different structures or sizes.

[0055] In other embodiments, depending on the different iodine samples, for example, the different detection wavelengths of water iodine and urine iodine may require different photoelectric detection modules, different reagents, and addition sequences. The fully automatic sampling device of any of the above schemes can be combined with different light sources and automated processes in the photoelectric detection modules to obtain a fully automatic analyzer that can detect a variety of different iodine samples.

[0056] Technical Effects

[0057] 1. The whole machine has a simple structure, no mechanical clamping claws, integrated digestion constant temperature design, low manufacturing cost, high operating reliability of the whole machine, and is convenient for product cost control and product quality control;

[0058] 2. Wide range of applications: compatible with comprehensive testing of urine iodine, salt iodine, and water iodine, meeting various standard testing methods in the fields of disease control and food, and one device can complete all tests;

[0059] 3. Good data stability: The present invention adopts more constant temperature and heat preservation designs, which makes the reaction temperature more consistent and the data results more repeatable and reproducible. The design of the converging external light path photoelectric detection module enables the LED with extremely small current to achieve high signal-to-noise ratio detection. The module has better thermal stability, fast data thermal stability, and small data drift.

[0060] 4. Designed for greater energy conservation and environmental protection: Independent flow paths for adding highly toxic reagents reduce the need for mixing and cross-piping rinses, reducing emissions and making the equipment more environmentally friendly. The equipment's excellent thermal insulation and constant-temperature heat recycling fully utilize heat, preventing it from spreading and losing, and improving the equipment's energy efficiency. The water supply and drainage pump design maximizes the recycling of constant-temperature water.

[0061] 5. Higher measurement efficiency and greater environmental adaptability: The system has added a refrigeration device. After digestion, the digestion temperature is quickly reduced to a constant temperature by the refrigeration device, avoiding the slow cooling, high water consumption, and inability to reach the specified temperature caused by excessively high ambient temperatures. The system has higher measurement efficiency and is capable of handling harsh environmental conditions. In contrast, the conventional water circulation method is to cool 100°C water to around 30°C. When the ambient temperature is too high, the cooling process takes a very long time and consumes a lot of water.

[0062] 6. The three-axis injection system uses three motion modules and a multi-functional injection needle to complete the reagent addition, mixing, sample transfer and measurement functions of non-through-hole positions in the entire experiment. Compared with the three-axis systems disclosed in "CN202020625727-Fully Automatic Urine Iodine and Water Iodine Analyzer" and "CN202010326714-Fully Automatic Urine Iodine and Water Iodine Analyzer and Analysis Method", there is no need for a manipulator to grab the sample tube, which effectively reduces the mechanical risk of grabbing and transferring failure, and the production cost is better; Existing defects: Beijing Baode uses a manipulator and needs to move the sample tube to the turbine for oscillation and mixing (the present invention does not require movement, and directly mixes through air to simplify the structure).

[0063] 7. The multifunctional injection needle adopts a different drop design. When the injection needle is inserted into the sample tube, the sample needle in the center is immersed in the liquid, while the first reagent needle and the second reagent needle on both sides of the sample needle are located above the liquid surface, which prevents the sample from contaminating the reagent pipeline and also prevents cross-contamination between reagent pipelines. The reagent needle is located below the liquid surface and can achieve liquid mixing by blowing bubbles, and can also achieve convenient transfer of the test solution by drawing. The use of ammonium persulfate solution and ammonium cerium sulfate solution in the determination of this project is time-exclusive. The present invention uses the technology of time-sharing multiplexing pipelines and the pipeline rinsing process to realize the reuse of injection needle pipelines. Two reagent needles can be used to achieve cross-contamination-free addition of multiple reagents.

[0064] 8. The integrated digestion constant temperature module integrates the functions of a metal bath and a water bath. Compared with the traditional split design, it saves more space and simplifies the number of temperature control components. The use of diaphragm pumps as water supply and drainage pumps can achieve rapid water replenishment and drainage. Compared with "CN202021205027-A New Iodine Analysis Device with Automatic Digestion", it can achieve dynamic drainage, preventing problems such as poor gravity drainage and low efficiency caused by water seals and air seals in the discharge pipeline. Compared with peristaltic pumps, diaphragm pumps do not require operators to regularly maintain pump tubes, making equipment maintenance easier. The parallel design of the water supply and drainage pumps not only meets the water supply and drainage needs of the equipment, but also realizes the recycling of constant temperature water compared to traditional designs, reducing the work of adding constant temperature water each time, saving energy and being efficient. The design of the circulating water pump in the module effectively improves the temperature uniformity of the entire system by establishing water circulation in the water bath. The design of the insulation sleeve in the module not only greatly reduces the heat radiation of the heating and insulation system, reduces the power consumption of the entire machine, and improves the system's ability to resist environmental changes, but also prevents other high-temperature failures of the equipment caused by thermal expansion.

[0065] 9. The multi-band photoelectric detection module adopts a low-power LED and photocell detection solution. Compared with the "CN201821797362-Multi-band Detection Colorimetric Cell and Water Quality Monitor" solution, the external light path aggregation design of this solution effectively improves the light source irradiation utilization rate, making the energy consumption of the entire LED power supply control system extremely low. It can not only reduce the thermal radiation of the photoelectric detection module and the drift of the entire photoelectric detection system, but also enable the system to quickly reach thermal stability equilibrium, thereby improving the system's ease of use and reliability.

[0066] 10. The multifunctional needle washing waste liquid pool adopts an integrated design. This module can not only realize the pollution-free cleaning of sample needles, but also realize the automatic overflow discharge of waste liquid. It can also collect the high-temperature wastewater generated by the integrated digestion constant temperature module during the water cooling process, and can also collect waste liquid during the detection process and waste liquid during the cleaning of reagent pipelines. It has a simple structure, low cost and comprehensive functions.

[0067] 11. The reagent injection component adopts a multi-channel time-sharing multiplexing design, which can not only realize the reagent adding function, but also realize the non-simultaneous addition of different reagents through the switching valve. The common liquid adding pump reduces the production cost. The present invention is also based on the actual use. Since arsenous acid (the main ingredient is arsenic) is a highly toxic and highly polluting reagent, a separate liquid adding pump is designed. Compared with "CN202021205027-A new iodine analysis device with automatic digestion", it can effectively reduce the arsenic pollution caused by the reagent switching, rinsing, and cleaning pipelines in the experimental link.

[0068] 12. The present invention adopts a water supply pump and a drainage pump in an alternating parallel design. The water outlet of the water supply pump is connected to the water inlet of the drainage pump and connected to the water supply and drainage interface of the water bath. The water inlet of the water supply pump is connected to the water outlet of the drainage pump and connected to the water tank outside the equipment. By turning on the water supply pump and drainage pump separately, the two functions of water supply and drainage can be achieved. This flow path design uses dynamic automatic drainage to prevent problems such as poor gravity drainage and low efficiency caused by water seals and air seals in the discharge pipeline. In addition, compared with peristaltic pumps, diaphragm pumps do not require operators to regularly maintain the pump tubes, making equipment maintenance easier.

[0069] 13. Since the water inlet and drainage are connected to the external water tank, the parallel design of the water supply and drainage pumps can not only meet the water supply and drainage needs of the equipment, but also realize the recycling of constant temperature water compared to the traditional design, reducing the waste caused by the discharge of constant temperature water as waste liquid each time, and saving energy and efficiency; the design of the circulating water pump in the module effectively improves the temperature uniformity of the entire system by constructing water circulation in the water bath. After actual testing, the temperature uniformity of the system is better than 0.1℃.

[0070] 14. In other embodiments, depending on the difference in iodine samples, for example, the different detection wavelengths of water iodine and urine iodine may require different photoelectric detection modules, different reagents, and addition sequences. The fully automatic sampling device of any of the above schemes can be combined with different light sources and automated processes in the photoelectric detection modules to obtain a fully automatic analyzer that can detect a variety of different iodine samples. BRIEF DESCRIPTION OF THE DRAWINGS

[0071] Figure 1 This is the overall structural outline of the present invention;

[0072] Figure 2 It is a schematic diagram of the structure of the three-axis injection system;

[0073] Figure 3 Schematic diagram of the multifunctional injection needle structure;

[0074] Figure 4 This is a structural diagram of the integrated digestion constant temperature module;

[0075] Figure 5 It is a schematic diagram of the structure of the multi-band photoelectric detection module;

[0076] Figure 6 This is a structural diagram of a multifunctional needle washing waste liquid pool;

[0077] Figure 7 Schematic diagram of the structure of the reagent injection component;

[0078] Figure 8 Schematic diagram of the structure of the multi-band photoelectric detection module.

[0079] Figure 1 The bid number is as follows:

[0080] 11: Three-axis injection module, 12: Multifunctional injection needle, 13: Integrated digestion constant temperature module, 14: Multifunctional needle washing waste liquid pool.

[0081] Figure 2 The bid number is as follows:

[0082] 21: X-axis module, 22: Y-axis module, 23: Z-axis module.

[0083] Figure 3 The bid number is as follows:

[0084] 31: sample needle, 32: first reagent needle, 33: second reagent needle.

[0085] Figure 4 The bid number is as follows:

[0086] 40: Sample tube, 41: Upper panel, 42: Fan, 43: Insulation board, 44: Heating element, 45: Water bath, 46: Heating rod, 47: Temperature sensor, 48: Temperature control module, 49: Circulating water pump, 50: Drain pump, 51: Water supply pump, 52: Water tank, 77: Water bath overflow interface

[0087] Figure 5 The bid number is as follows:

[0088] 53: Circulating colorimetric cell, 54-1: First condensing lens, 54-2: Second condensing lens, 55: LED lamp beads, 56: Light source board, 57: Rotating motor, 58: Photocell detection board, 59: Module communication interface.

[0089] Figure 6 The bid number is as follows:

[0090] 60: pure water tank, 61: needle washing pump, 62: needle washing pool entrance, 63: needle washing pool, 64: overflow port, 65: first waste liquid chamber, 66: water bath overflow inner interface, 67: connecting port, 68: second waste liquid chamber, 69: first waste liquid interface, 70: second waste liquid interface.

[0091] Figure 7 The bid number is as follows:

[0092] 71: first reagent container, 72: second reagent container, 73: third reagent container, 74: switching valve, 75: first liquid adding pump, 76: second liquid adding pump, 77: water bath overflow external interface. DETAILED DESCRIPTION

[0093] In order to make the technical means, creative features, objectives and effects of the invention easier to understand, the present invention is further described below with reference to specific illustrations.

[0094] Example 1: Structure of a fully automatic iodine analyzer

[0095] like Figure 1-3 As shown, a fully automatic sampling device for multiple iodine samples includes a base, a three-axis sampling module 11, a three-axis sampling module 12, an integrated digestion constant temperature module 13, a reagent sampling module, and a pumping circulation module, wherein:

[0096] (1) The base is the base of the analyzer, and the upper surface is provided with a sample table for placing samples, and the interior is provided with an integrated digestion constant temperature module 13, a photoelectric detection module, a needle washing module, a reagent injection module, and a pumping circulation module;

[0097] (2) A three-axis sample injection module 11 located above the base includes three modules in the X (horizontal) direction, the Y (front and back) direction, and the Z (up and down) direction. The end of the Z module is fixedly connected to the three-axis sample injection module 12. The three-axis sample injection module 11 can realize the programmable displacement of the three-axis sample injection module 12 in the up, down, left, right, front and back directions.

[0098] (3) The three-axis injection module 12 is composed of a first reagent needle 32, a sample needle 31, and a second reagent needle 33 from left to right. The three needles are integrally formed using bonding / welding technology, wherein the end of the middle sample needle 31 protrudes from the ends of the first and second reagent needles 33 on both sides, so that when the central sample needle 31 is immersed in the liquid, the first reagent needles 32 and the second reagent needles 33 on both sides are located above the liquid surface, which can prevent the sample from contaminating the reagent pipeline and prevent cross-contamination between reagent pipelines.

[0099] In addition, the base surface is also provided with a multifunctional needle washing waste liquid pool 14. When the three-axis injection module completes the injection, the three-axis mobile injection module can move the injection needle to the waste liquid pool for cleaning the injection needle.

[0100] like Figure 4 As shown, the main body of the integrated digestion constant temperature module 13 is located inside the base, and includes a sample tube 40, a heating body 44, a temperature sensor 47, a temperature control module 48, a water bath 45, and an air cooling channel.

[0101] The sample tube 40 is located inside the vertically downward base of the triaxial sampling module 12, with its lower portion being located in a heating element 44 and its upper portion being located in an air-cooling channel running through both ends of the base. A temperature sensor 47 is located inside the heating element 44, and a water bath 45 is located outside the heating element 44 to provide a constant temperature environment for the sample tube 40. The bottom of the water bath 45 is provided with multiple water supply and drainage interfaces. A temperature sensor 47 is also located outside the base.

[0102] The pumping circulation module includes a water supply pump 51, a drainage pump 50, and a circulation pump 49, wherein the water supply pump 51 and the drainage pump 50 are arranged alternately in parallel, that is, the water outlet of the water supply pump 51 is connected with the water inlet of the drainage pump 50 and connected to a water supply and drainage interface of the water bath 45, and the water inlet of the water supply pump 51 is connected with the water outlet of the drainage pump 50 and connected to the water tank outside the equipment. By opening the water supply pump 51 and the drainage pump 50 separately, the water bath 45 can be supplied with water and drained; the water inlet and water outlet of the circulation pump 49 are respectively connected to different water supply and drainage interfaces of the water bath 45, so that the water in the water bath 45 circulates as needed to maintain a constant temperature environment.

[0103] Fans 42 are provided at both ends of the air cooling channel of the digestion constant temperature module. When the fan 42 is turned on, an air cooling zone is formed to achieve sample condensation and reflux during the digestion process and reduce sample digestion volatilization. When the fan 42 is turned off, a constant temperature zone is formed.

[0104] A heat-insulating plate 43 is provided between the air-cooling channel and the water bath 45. A heat-insulating sleeve is provided on the outer surface of the water bath 45. A heating element 44 is made of a heat-conducting material and has a heating rod 46 inside.

[0105] For the detection process that does not require digestion treatment such as salt iodine, under the function of the automatic controller, the integrated digestion constant temperature module 13 only has the temperature control module 48 to process the water bath 45, and no air cooling channel is needed to maintain a constant temperature environment during the detection process.

[0106] For the detection process of urine iodine and other substances that require digestion treatment, a cooling device can be connected in series in the flow path of the circulation pump 49 of the pumping circulation module ( Figure 4 Not shown). The cooling device can be an existing conventional cooling device, such as a semiconductor refrigerator (CN2012103472518, or CN2020106676009). When the urine iodine sample is detected, the automatic controller ( Figure 4 The cooling module (not shown) is activated during the water bath thermostating after digestion, rapidly cooling the hot water to a constant temperature. This improves system efficiency and reduces process water usage. Because the cooling device is connected in series to the flow path of the circulating pump 49 and regulated by the automated controller, it does not affect the sampling and detection of water iodine and salt iodine by the sample introduction device when not activated.

[0107] like Figure 7-8 As shown, the reagent injection module includes a first reagent container 71, a second reagent container 72 and / or a third reagent container 73, a second liquid adding pump 76 and a first liquid adding pump 75 for driving the first, second and / or third reagents into the first or second reagent needle 33, and a transfer pump 80 for driving the sample or air into the sample needle 31. When the sample needle 31 adds the sample to be tested into the sample tube 40, and / or the first or second reagent needle 33 located above the liquid surface adds the reagent into the sample tube 40, the sample needle 31 located below the liquid surface is driven by the transfer pump 80 to allow gas to enter the sample tube 40 through the sample needle 31, thereby achieving gas mixing and stirring, and realizing contactless addition of the first and second reagents, thereby reducing contact contamination.

[0108] In addition, the second reagent container 72 and the third reagent container 73 are designed in parallel, and a switching valve 74 is provided at the parallel intersection, so that the second liquid adding pump 76 drives the second reagent or the third reagent into the first reagent needle 32, and the first liquid adding pump 75 drives the first reagent into the second reagent needle 33, thereby achieving the addition of different reagents for different iodine samples.

[0109] like Figure 5-6 and Figure 8As shown, it is used to be assembled with the above-mentioned sample injection device to form a cleaning module and a multi-band photoelectric detection module of a multifunctional fully automatic iodine element analyzer.

[0110] Figure 5 As shown, the multi-band photoelectric detection module is provided with a module communication interface 59, a rotating motor 57, a rotating light source board 56, an LED lamp bead 55, a first focusing lens 54-1, a circulation colorimetric cell 53, a second focusing lens 54-2, and a photoelectric detection board 58 in sequence according to the direction of travel of the light path. The first focusing lens 54-1 and the second focusing lens 54-2 are provided at both ends of the circulation colorimetric cell 53, and the upper end is provided with a passage for receiving the sample solution to be tested from the sample needle 31, as well as a passage for connecting to the first waste liquid interface 69.

[0111] The transfer pump 80 (see FIG. Figure 8 ), the sample solution to be tested in the sample tube 40 is drawn into the circulation colorimetric cell 53 through the sample needle 31. The rotating motor 57 rotates the LED lamp bead 55 of the preset wavelength to align with the light path by rotating the light source plate 56. The light emitted by the light source passes through the first focusing lens 54-1, the circulation colorimetric cell 53, and the second focusing lens 54-2 until it is focused on the photocell detection board 58. The photocell detection board 58 converts the detected light signal into an electrical signal, which is transmitted to the main control board and computer via the module communication interface 59. The solution after passing through the circulation colorimetric cell 53 enters the first waste liquid interface 69 of the multifunctional needle washing waste liquid tank 14 through the transfer pump 80. The waste liquid flows downward due to gravity and is discharged from the equipment through the second waste liquid interface 70.

[0112] like Figure 6 As shown, the analyzer also includes a cleaning module, which includes an integrated multifunctional needle washing waste liquid pool 14 and a liquid transfer pipeline, wherein the multifunctional needle washing waste liquid pool includes a pure water tank 60, a needle washing pump 61, a needle washing pool inlet 62, a needle washing pool 63, an overflow port 64, a first waste liquid chamber 65, a second waste liquid chamber 68, a first waste liquid interface 69, and a second waste liquid interface 70 in order of connection, wherein the needle washing pool 63 is connected to the first waste liquid chamber 65 through the overflow port 64 at the top, and the first waste liquid chamber 65 is connected to the bottom of the second waste liquid chamber 68 through the connecting port 67 at the bottom, the first waste liquid interface 69 is located at the upper part of the second waste liquid chamber 68, and the second waste liquid interface 70 is located at the lower part of the second waste liquid chamber 68.

[0113] After the measurement is completed, the needle washing pump 61 is turned on, and the pure water in the pure water tank 60 is injected into the needle washing pool 63 through the needle washing pool inlet 62. The three-axis sampling module 11 is moved so that the three-axis sampling module 12 is inserted into the needle washing pool 63 to complete the cleaning; the sewage flows into the first waste liquid chamber 65 through the overflow port 64, and is discharged from the second waste liquid interface 70 through the connecting port at the bottom.

[0114] The fully automatic sample injection device, cleaning module and / or multi-band photoelectric detection module are all modularly designed and can replace the existing iodine analyzer to obtain iodine analyzers of different structures or sizes.

[0115] Among them, according to the different iodine samples, for example, the detection wavelengths of water iodine and urine iodine are inconsistent, which requires different photoelectric detection modules, different reagents and addition sequences. The fully automatic sampling device of any of the above schemes can be combined with different light sources and automated processes in the photoelectric detection module to obtain a fully automatic analyzer that can detect a variety of different iodine samples.

[0116] Figure 1 It is also an overall schematic diagram of the fully automatic sampling device / analyzer. The device or analyzer, in conjunction with an automated controller and related programs, controls the start-up of the digestion constant temperature module and the order of adding different reagents, thereby achieving multiplexing of the sampling needle pipeline and analyzing different water iodine, urine iodine, and salt iodine samples.

[0117] Example 2: Working principle of automatic analysis of urine iodine detection according to the present invention

[0118] like Figure 3-4 As shown, the sample tube 40 is placed in the integrated digestion constant temperature module 13, the X-axis module 21 and the Y-axis module 22 of the three-axis injection system 11 are moved so that the multifunctional injection needle 12 is located above the sample tube 40, and the Z-axis module 23 is moved to insert the multifunctional injection needle 12 into the sample tube 40. The reagent in the second reagent container 72 is fed through the first reagent needle 32 (see FIG. 1 ) by the cooperation of the first liquid adding pump 75 and the switching valve 74. Figure 7 ), add the sample tube 40, and at the same time the transfer pump 80 rotates, draws air from the multifunctional needle washing waste liquid pool 14 through the circulation colorimetric pool 53 and the sample needle 31, and injects it into the sample tube 40 to achieve the effect of stirring and mixing. Figure 8 .

[0119] A temperature control module 48 is set to make the heating rod 46 in the heating body 44 work, and a temperature sensor 47 is used to collect the temperature in real time, so that the heating body 44 reaches the digestion temperature required by the standard. The fans 42 at both ends of the air cooling channel are turned on, so that the upper panel 41 and the thermal insulation board 43 form an air cooling area, so that the sample can be condensed and refluxed during the digestion process, reducing the volatilization of the sample digestion. Figure 4 .

[0120] After the prescribed digestion time, the temperature control module 48 is set to the constant temperature required by the standard, and the constant temperature circulating water in the water tank 52 is injected into the water bath 45 through the water supply pump 51. The excess water enters the first waste liquid chamber 65 through the water bath overflow external interface 77 and connects to the water bath overflow internal interface 66. It passes through the connecting port 67 and is finally discharged from the device through the second waste liquid interface 70. When the temperature of the heating body 44 is reduced to the preset temperature by adding a certain amount of water, the water supply is stopped and the circulating water pump 49 is turned on to circulate the constant temperature circulating water in the water bath 44, further improving the temperature uniformity. Figure 4 and Figure 6 Among them, the cooling module can be turned on by the automatic controller, which can quickly cool the high-temperature water to a constant temperature, improving system efficiency and reducing process water consumption.

[0121] Move the X-axis module 21 and the Y-axis module 22 of the three-axis injection system 11 so that the multifunctional injection needle 12 is located above the sample tube 40. Move the Z-axis module 23 and insert the multifunctional injection needle 12 into the sample tube 40. The reagent in the first reagent container 71 is added to the sample tube 40 through the second reagent needle 33 by the second liquid adding pump 76. At the same time, the transfer pump 80 rotates to draw air from the multifunctional needle washing waste liquid pool 14 through the circulation colorimetric cell 53 and the sample needle 31 and inject it into the sample tube 40 to achieve the effect of stirring and mixing. Let it stand for a certain time according to the standard requirements. Figure 7 .

[0122] Move the X-axis module 21 and the Y-axis module 22 of the three-axis injection system 11 so that the multifunctional injection needle 12 is located above the sample tube 40. Move the Z-axis module 23 and insert the multifunctional injection needle 12 into the sample tube 40. The reagent in the third reagent container 73 is added to the sample tube 40 through the first reagent needle 32 by the cooperation of the first liquid adding pump 75 and the switching valve 74. At the same time, the transfer pump 80 rotates to draw air from the multifunctional needle washing waste liquid pool 14 through the circulation colorimetric cell 53 and the sample needle 31 and inject it into the sample tube 40 to achieve the effect of stirring and mixing. Let it stand for a certain time according to the standard requirements. Figure 7 .

[0123] By rotating the transfer pump 80, the sample solution in the sample tube 40 is drawn into the circulation colorimetric cell 53 through the sample needle 31. Figure 5In the multi-band photoelectric detection module, the rotating motor 57 rotates the light source board 56 to rotate the LED lamp bead 55 of the specified wavelength of the measurement item to align with the light path. The light emitted by the light source passes through the first focusing lens and is focused in the circulation colorimetric cell 53. The light after passing through the circulation colorimetric cell 53 passes through the second focusing lens and is focused on the photocell detection board 58. The photocell detection board 58 converts the detected light signal into an electrical signal, which is transmitted to the main control board and the computer through the module communication interface 59. The solution after passing through the circulation colorimetric cell 53 enters the first waste liquid interface 69 of the multi-functional needle washing waste liquid pool 14 through the transfer pump 80. The waste liquid flows downward due to gravity and is discharged from the equipment through the second waste liquid interface 70. Figure 8 .

[0124] After the measurement is completed, turn on the needle washing pump 61, and inject the pure water in the pure water tank 60 into the needle washing pool 63 through the needle washing pool inlet 62 at a certain rate. Move the X-axis module 21 and the Y-axis module 22 of the three-axis injection system 11 so that the multifunctional injection needle 12 is located above the needle washing pool 63. Insert the multifunctional injection needle 12 into the needle washing pool 63. The sewage remaining on the outer wall of the multifunctional injection needle 12 is located above the needle washing pool 63. As the pure water is continuously injected, the sewage will flow into the first waste liquid chamber 65 through the overflow port 64, through the connecting port 67, and finally discharged from the device through the second waste liquid interface 70. Turn the transfer pump 80 to draw the pure water in the needle washing pool into the circulation colorimetric cell 53 through the sample needle 31, through the transfer pump 80 and the first waste liquid interface 69, and finally discharged from the device through the second waste liquid interface 70, so as to achieve the cleaning of the inner wall of the multifunctional injection needle 12. Figure 6 .

[0125] Move the X-axis module 21 and the Y-axis module 22 of the three-axis injection system 11 so that the multifunctional injection needle 12 is located above the first waste liquid chamber 65, insert the multifunctional injection needle 12 into the first waste liquid chamber 65, and rotate the transfer pump 80 to draw air from the multifunctional needle washing waste liquid pool 14 through the circulation colorimetric cell 53 and the sample needle 31, and inject it into the sample tube 40, thereby emptying the sample tube.

[0126] The circulating water pump 49 is turned off and the drain pump 50 is turned on to discharge the constant temperature circulating water in the water bath 45 into the water tank 52 to realize water recycling.

[0127] Example 3: Working principle of automatic analysis of water iodine detection according to the present invention

[0128] like Figure 3-4As shown, the sample tube 40 is placed in the integrated digestion constant temperature module 13, the X-axis module 21 and the Y-axis module 22 of the three-axis injection system 11 are moved so that the multifunctional injection needle 12 is located above the sample tube 40, the Z-axis module 23 is moved, and the multifunctional injection needle 12 is inserted into the sample tube 40. The reagent in the second reagent container 72 is passed through the first reagent needle 32 (see FIG. 1 ) by the cooperation of the first liquid addition pump 75 and the switching valve 74. Figure 7 ), add the sample tube 40, and at the same time the transfer pump 80 rotates, draws air from the multifunctional needle washing waste liquid pool 14 through the circulation colorimetric pool 53 and the sample needle 31, and injects it into the sample tube 40 to achieve the effect of stirring and mixing. Let it stand for a certain time according to the standard requirements. Figure 8 .

[0129] Move the X-axis module 21 and the Y-axis module 22 of the three-axis injection system 11 so that the multifunctional injection needle 12 is located above the sample tube 40. Move the Z-axis module 23 to insert the multifunctional injection needle 12 into the sample tube 40. The reagent in the first reagent container 71 is added to the sample tube 40 through the second reagent needle 33 by the second liquid adding pump 76. At the same time, the transfer pump 80 rotates to draw air from the multifunctional needle washing waste liquid pool 14 through the circulation colorimetric cell 53 and the sample needle 31 and inject it into the sample tube 40 to achieve the effect of stirring and mixing (see Figure 7 ), set 48 temperature control module, make 46 heating rod work, and use 47 temperature sensor to collect temperature in real time, set 44 heating body to constant temperature required by standard, and let it stand for a certain time according to standard requirements. Figure 4 .

[0130] Move the X-axis module 21 and the Y-axis module 22 of the three-axis injection system 11 so that the multifunctional injection needle 12 is located above the sample tube 40. Move the Z-axis module 23 and insert the multifunctional injection needle 12 into the sample tube 40. The reagent in the third reagent container 73 is added to the sample tube 40 through the first reagent needle 32 by the cooperation of the first liquid adding pump 75 and the switching valve 74. At the same time, the transfer pump 80 rotates to draw air from the multifunctional needle washing waste liquid pool 14 through the circulation colorimetric cell 53 and the sample needle 31 and inject it into the sample tube 40 to achieve the effect of stirring and mixing. Let it stand for a certain time according to the standard requirements. Figure 7 .

[0131] By rotating the transfer pump 80, the sample solution in the sample tube 40 is drawn into the circulation colorimetric cell 53 through the sample needle 31. Figure 5In the multi-band photoelectric detection module, the rotating motor 57 rotates the light source board 56 to rotate the LED lamp bead 55 of the specified wavelength of the measurement item to align with the light path. The light emitted by the light source passes through the first focusing lens and is focused in the circulation colorimetric cell 53. The light after passing through the circulation colorimetric cell 53 passes through the second focusing lens and is focused on the photocell detection board 58. The photocell detection board 58 converts the detected light signal into an electrical signal, which is transmitted to the main control board and the computer through the module communication interface 59. The solution after passing through the circulation colorimetric cell 53 enters the first waste liquid interface 69 of the multi-functional needle washing waste liquid pool 14 through the transfer pump 80. The waste liquid flows downward due to gravity and is discharged from the equipment through the second waste liquid interface 70. Figure 8 .

[0132] After the measurement is completed, turn on the needle washing pump 61, and inject the pure water in the pure water tank 60 into the needle washing pool 63 through the needle washing pool inlet 62 at a certain rate. Move the X-axis module 21 and the Y-axis module 22 of the three-axis injection system 11 so that the multifunctional injection needle 12 is located above the needle washing pool 63. Insert the multifunctional injection needle 12 into the needle washing pool 63. The sewage remaining on the outer wall of the multifunctional injection needle 12 is located above the needle washing pool 63. As the pure water is continuously injected, the sewage will flow into the first waste liquid chamber 65 through the overflow port 64, through the connecting port 67, and finally discharged from the device through the second waste liquid interface 70. Turn the transfer pump 80 to draw the pure water in the needle washing pool 62 into the circulation colorimetric cell 53 through the sample needle 31, through the transfer pump 80 and the first waste liquid interface 69, and finally discharged from the device through the second waste liquid interface 70, so as to achieve the cleaning of the inner wall of the multifunctional injection needle 12. Figure 6 .

[0133] Move the X-axis module 21 and the Y-axis module 22 of the three-axis injection system 11 so that the multifunctional injection needle 12 is located above the first waste liquid chamber 65, insert the multifunctional injection needle 12 into the first waste liquid chamber 65, and rotate the transfer pump 80 to draw air from the multifunctional needle washing waste liquid pool 14 through the circulation colorimetric cell 53 and the sample needle 31, and inject it into the sample tube 40, thereby emptying the sample tube.

[0134] The circulating water pump 49 is turned off and the drain pump 50 is turned on to discharge the constant temperature circulating water in the water bath 45 into the water tank 52 to realize water recycling.

[0135] Compared with the urine iodine detection in Example 2, the water iodine detection process in Example 3 is mainly different in that the digestion process is omitted, but the constant temperature heating process is still retained.

[0136] Example 4: Automatic analysis working principle of the present invention during salt iodine detection

[0137] Considering that the reagents added for salt iodine testing are different from those for urine iodine, and that a highly toxic arsenic-containing reagent needs to be added, a different order of reagent addition needs to be designed. The workflow is as follows:

[0138] Place the sampled sample tube 40 in the integrated digestion constant temperature module 13. Move the X-axis module 21 and Y-axis module 22 of the three-axis injection system 11 so that the multifunctional injection needle 12 is located above the sample tube 40. Move the Z-axis module 23 to insert the multifunctional injection needle 12 into the sample tube 40. The reagent in the second reagent container 72 is added to the sample tube 40 through the first reagent needle 32 through the cooperation of the first liquid adding pump 75 and the switching valve 74. Unlike Example 2, the reagent in the first reagent container 71 is also added to the sample tube 40 through the second reagent needle 33 through the second liquid adding pump 76. At the same time, the transfer pump 80 rotates, drawing air from the multifunctional needle washing waste liquid pool 14 through the circulation colorimetric cell 53 and the sample needle 31, and then injecting it into the sample tube 40 to achieve the effect of stirring and mixing.

[0139] Different from Example 2, the X-axis module 21 and the Y-axis module 22 of the three-axis injection system 11 are moved so that the multi-function injection needle 12 is located above the first waste liquid chamber 65, and the multi-function injection needle 12 is inserted into the first waste liquid chamber 65. The reagent in the third reagent container 73 is discharged into the first waste liquid chamber 65 through the first reagent needle 32 through the cooperation of the first liquid adding pump 75 and the switching valve 74, so that the third reagent fills the pipeline and achieves the purpose of rinsing the pipeline.

[0140] After the third reagent rinse pipeline, move the X-axis module 21 and the Y-axis module 22 of the three-axis injection system 11 again so that the multifunctional injection needle 12 is located above the sample tube 40, move the Z-axis module 23, and insert the multifunctional injection needle 12 into the sample tube 40. Through the cooperation of the first liquid adding pump 75 and the switching valve 74, continue to add the reagent in the third reagent container 73 to the sample tube 40 through the first reagent needle 32, and at the same time, rotate the transfer pump 80 to draw air from the multifunctional needle washing waste liquid pool 14 through the circulation colorimetric pool 53 and the sample needle 31, and inject it into the sample tube 40 to achieve the effect of stirring and mixing.

[0141] By rotating the transfer pump 80, the sample solution in the sample tube 40 is drawn into the circulation colorimetric cell 53 through the sample needle 31. Figure 5 In the multi-band photoelectric detection module, the rotating motor 57 rotates the light source board 56 to rotate the LED lamp bead 55 of the specified wavelength of the measurement item to align with the light path. The light emitted by the light source passes through the first focusing lens and is focused in the circulation colorimetric cell 53. The light after passing through the circulation colorimetric cell 53 passes through the second focusing lens and is focused on the photocell detection board 58. The photocell detection board 58 converts the detected light signal into an electrical signal, which is transmitted to the main control board and the computer through the module communication interface 59. The solution after passing through the circulation colorimetric cell 53 enters the first waste liquid interface 69 of the multi-functional needle washing waste liquid pool 14 through the transfer pump 80. The waste liquid flows downward due to gravity and is discharged from the equipment through the second waste liquid interface 70. Figure 8.

[0142] After the measurement is completed, turn on the needle washing pump 61, and inject the pure water in the pure water tank 60 into the needle washing pool 63 through the needle washing pool inlet 62 at a certain rate. Move the X-axis module 21 and the Y-axis module 22 of the three-axis injection system 11 so that the multifunctional injection needle 12 is located above the needle washing pool 63. Insert the multifunctional injection needle 12 into the needle washing pool 63. The sewage remaining on the outer wall of the multifunctional injection needle 12 is located above the needle washing pool 63. As the pure water is continuously injected, the sewage will flow into the first waste liquid chamber 65 through the overflow port 64, through the connecting port 67, and finally discharged from the device through the second waste liquid interface 70. Turn the transfer pump 80 to draw the pure water in the needle washing pool 62 into the circulation colorimetric cell 53 through the sample needle 31, through the transfer pump 80 and the first waste liquid interface 69, and finally discharged from the device through the second waste liquid interface 70, so as to achieve the cleaning of the inner wall of the multifunctional injection needle 12. Figure 6 .

[0143] Move the X-axis module 21 and the Y-axis module 22 of the three-axis injection system 11 so that the multifunctional injection needle 12 is located above the first waste liquid chamber 65, insert the multifunctional injection needle 12 into the first waste liquid chamber 65, and rotate the transfer pump 80 to draw air from the multifunctional needle washing waste liquid pool 14 through the circulation colorimetric cell 53 and the sample needle 31, and inject it into the sample tube 40, thereby emptying the sample tube.

[0144] The circulating water pump 49 is turned off and the drain pump 50 is turned on to discharge the constant temperature circulating water in the water bath 45 into the water tank 52 to realize water recycling.

[0145] As can be seen from Example 4, although the detection of salt iodine does not require a digestion process and an obvious constant temperature process, the automated addition and detection of salt iodine can be completed on the basis of the detection of urine iodine by simply changing the order of reagent addition through the automatic controller.

[0146] In summary, based on the various functional modules required for detecting urine iodine, the present invention can realize the process of detecting urine iodine, water iodine and salt iodine by one instrument by optimizing the program and addition sequence, and realize automatic sample addition and cleaning in the whole process.

Claims

1. A fully automatic sampling device for multiple iodine samples, which can fully automatically sample water iodine, urine iodine, and salt iodine samples, including a base, a three-axis sampling module, a multifunctional sampling needle, an integrated digestion and constant temperature module, a reagent sampling module, and a pumping circulation module, characterized in that: The base is the base of the analyzer, with a sample table on the upper surface for placing samples, and an integrated digestion and constant temperature module, photoelectric detection module, needle washing module, reagent injection module, and pumping circulation module inside; The three-axis injection module located above the base includes three modules in the X, Y, and Z directions. The end of the Z module is fixedly connected to the multi-function injection needle. The three-axis injection module can realize the programmable displacement of the multi-function injection needle in the up, down, left, right, front, and back directions. The multifunctional injection needle is composed of a first reagent needle, a sample needle, and a second reagent needle from left to right. The three needles are integrally formed using gluing / welding technology. The end of the central sample needle protrudes from the ends of the first and second reagent needles on both sides. When the central sample needle is immersed in the liquid, the first and second reagent needles on both sides are above the liquid surface, which can prevent sample contamination of the reagent pipeline and prevent cross contamination between reagent pipelines. The main body of the integrated digestion constant temperature module is located inside the base and includes a sample tube, a heating element, a temperature sensor temperature control module, a water bath, and an air cooling channel. The sample tube is located inside the base, with the multifunctional injection needle pointing vertically downward. The lower part is set in the heating element, and the upper part is set in the air cooling channel running through both ends of the base. A temperature sensor is installed inside the heating element, and a water bath is installed outside to provide a constant temperature environment for the sample tube. The bottom of the water bath is equipped with multiple water supply and drainage interfaces. In addition, a temperature sensor is installed outside the base. The reagent injection module includes a first reagent container, a second reagent container and / or a third reagent container, and a second liquid adding pump and a first liquid adding pump for driving the first, second and / or third reagent into the first or second reagent needle, and a transfer pump for driving the sample or air into the sample needle; The pumping circulation module includes a water supply pump, a drainage pump, and a circulation pump, wherein the water supply pump and the drainage pump are alternately arranged in parallel, that is, the water outlet of the water supply pump is connected to the water inlet of the drainage pump and connected to a water supply and drainage interface of the water bath, the water inlet of the water supply pump is connected to the water outlet of the drainage pump and connected to the water tank outside the equipment, and the water supply and drainage of the water bath can be achieved by opening the water supply pump and the drainage pump separately; the water inlet and outlet of the circulation pump are respectively connected to different water supply and drainage interfaces of the water bath, so that the water in the water bath circulates as needed to maintain a constant temperature environment; and, A multifunctional needle washing waste liquid pool, so that the multifunctional injection needle is transferred to the waste liquid pool for cleaning after adding the sample; and Fans are provided at both ends of the air cooling channel of the digestion constant temperature module, so that when the fans are turned on, an air cooling zone is formed to achieve sample condensation and reflux during the digestion process and reduce sample volatilization, while a constant temperature zone is formed when the fans are turned off; and The heating body is made of heat-conducting material and has a heating rod inside.

2. The device according to claim 1, characterized in that: When the sample needle adds the sample to be tested to the sample tube, and / or the first or second reagent needle located above the liquid surface adds the reagent to the sample tube, the sample needle located below the liquid surface is driven by the transfer pump, and the gas enters the sample tube through the sample needle, thereby achieving gas mixing and stirring, and realizing contactless addition of the first and second reagents, reducing contact contamination.

3. The device according to claim 2, characterized in that: A heat-insulating plate is provided between the air-cooling channel and the water bath, and a heat-insulating cover is provided on the outer surface of the water bath.

4. The device according to any one of claims 1 to 3, characterized in that: The second reagent container and the third reagent container are designed in parallel, and a switching valve is provided at the parallel intersection, so that the second liquid adding pump drives the second reagent or the third reagent into the first reagent needle, and the first liquid adding pump drives the first reagent into the second reagent needle, thereby achieving the addition of different reagents for different iodine samples.

5. The device according to claim 4, characterized in that: The fully automatic sampling device, combined with the automated controller and related programs, realizes the reuse of sampling needle pipelines and the analysis of different water iodine, urine iodine and salt iodine samples by controlling the start-up of the digestion constant temperature module and the order of adding different reagents.

6. The device according to claim 5, characterized in that: A cooling device can be connected in series in the flow path of the circulation pump of the pumping circulation module. When detecting urine iodine samples, the automatic controller will turn on the cooling module when the water bath is kept at a constant temperature after digestion, which can quickly cool the high-temperature water to a constant temperature, thereby improving system efficiency and reducing process water consumption.

7. A multifunctional fully automatic iodine element analyzer, characterized in that: The analyzer comprises the fully automatic sample injection device according to any one of claims 1 to 6, a cleaning module, and a multi-band photoelectric detection module.

8. The analyzer according to claim 7, characterized in that: The cleaning module includes an integrated multifunctional needle washing waste liquid pool and a liquid transfer pipeline, wherein the multifunctional needle washing waste liquid pool includes a pure water tank, a needle washing pump, a needle washing pool inlet, a needle washing pool, an overflow port, a first waste liquid chamber, a second waste liquid chamber, a first waste liquid port, and a second waste liquid port in order of connection, wherein the needle washing pool is connected to the first waste liquid chamber through the overflow port at the top, the first waste liquid chamber is connected to the bottom of the second waste liquid chamber through the connecting port at the bottom, the first waste liquid port is located at the upper part of the second waste liquid chamber, and the second waste liquid port is located at the lower part of the second waste liquid chamber.

9. The analyzer according to claim 8, characterized in that: The multi-band photoelectric detection module is provided with a module communication interface, a rotating motor, a rotating light source board, an LED lamp bead, a first focusing lens, a circulation colorimetric cell, a second focusing lens, and a photoelectric detection board in sequence according to the direction of travel of the light path. The first and second focusing lenses are provided at both ends of the circulation colorimetric cell, and the upper end is provided with a passage for receiving the sample solution to be tested from the sample needle, as well as a passage connected to the first waste liquid port.

10. The analyzer according to claim 8 or 9, characterized in that: The transfer pump provided on the passage connecting the circulation colorimetric cell and the first waste liquid port draws the sample solution to be tested in the sample tube into the circulation colorimetric cell through the sample needle. The rotating motor rotates the light source board to rotate the LED lamp beads of the preset wavelength to align with the light path. The light emitted by the light source passes through the first condensing lens, the circulation colorimetric cell, and the second condensing lens until it is focused on the photocell detection board. The photocell detection board converts the detected light signal into an electrical signal, which is transmitted to the main control board and the computer through the module communication interface.

11. The analyzer according to claim 10, characterized in that: The solution after passing through the circulation colorimetric cell enters the first waste liquid interface of the multifunctional needle washing waste liquid pool through the transfer pump. The waste liquid flows downward due to gravity and is discharged from the equipment through the second waste liquid interface.

12. The analyzer according to claim 11, characterized in that: After the measurement is completed, the needle washing pump is turned on, and the pure water in the pure water tank is injected into the needle washing pool through the needle washing pool inlet. The three-axis injection module is moved so that the multifunctional injection needle is inserted into the needle washing pool to complete the cleaning. The wastewater flows into the first waste liquid chamber through the overflow port and is discharged from the second waste liquid interface through the connecting port at the bottom.

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