Integrated full-scene adaptive total phosphorus rapid detection platform and analysis method

Abstract

The invention relates to an integrated full-scene adaptive total phosphorus rapid detection platform, which comprises a raw water collection module, a sample digestion module, a sample introduction reaction module and a detection module, the raw water collection module comprises an automatic sample injector capable of automatically switching a plurality of sample tubes and / or online water samples to collect raw water; the sample digestion module comprises sulfuric acid mixed with a sample, a heating reactor, potassium persulfate mixed with a mixed solution and an ultraviolet digestion device, and the sample introduction reaction module comprises a color developing agent mixed with the sample subjected to ultraviolet digestion, ascorbic acid mixed with the mixed solution and a heating reactor. The detection module comprises a flow cell of a final reaction product and a detector, and a plurality of modules of raw water collection, sample digestion, sample introduction reaction, detection and the like are integrated into a whole, so that full-process automatic operation from raw water collection to final detection result output is realized.

Description

Technical Field

[0001] This application relates to the technical field of water quality detection, specifically to the technical field of an integrated full-scenario adaptable total phosphorus rapid detection platform and analysis method. Background Art

[0002] In the field of environmental monitoring, the determination of total phosphorus content is crucial for evaluating water quality conditions, as phosphorus is one of the main elements causing water eutrophication. The ammonium molybdate spectrophotometry, as a classic and widely accepted method, is commonly used in total phosphorus detection. However, the traditional ammonium molybdate spectrophotometry usually requires complex sample pretreatment steps, which are not only time-consuming but also limit its application in on-site rapid detection. In addition, this method has high requirements for the professional skills of operators, and errors are easily introduced due to human factors, affecting the accuracy of the results.

[0003] At the same time, the current detection devices on the market either focus on high-precision measurement in the laboratory environment or on online monitoring in specific scenarios, and it is difficult to achieve full-scenario adaptation that is compatible with both offline and online. Therefore, there is a lack of an integrated solution that can flexibly adapt to the requirements of different application scenarios while ensuring the detection speed and accuracy. Summary of the Invention

[0004] In view of the above problems, this application proposes an integrated full-scenario adaptable total phosphorus rapid detection platform and analysis method, which utilizes the principle of Flow Injection Analysis (FIA) and combines the optimization of ammonium molybdate spectrophotometry to overcome the limitations of the existing technology and provide users with more convenient and efficient total phosphorus detection services.

[0005] To achieve the above object, this application adopts the following technical solutions:

[0006] In the first aspect, this application provides an integrated full-scenario adaptable total phosphorus rapid detection platform, including a raw water collection module, a sample digestion module, a sample injection and reaction module, and a detection module;

[0007] The raw water collection module includes an auto-sampler that can automatically switch between multiple sample tubes and / or online water samples for raw water collection and a peristaltic pump;

[0008] The sample digestion module includes sulfuric acid that is mixed with the samples transported by the raw water collection module through a tee, a peristaltic pump for pumping the sulfuric acid, and a heating reactor for the mixed solution thereof, potassium persulfate that is mixed with the mixed solution transported by the heating reactor, a peristaltic pump for pumping the potassium persulfate, and an ultraviolet digestion device for the mixed solution thereof;

[0009] The sample injection and reaction module includes a color reagent for mixing the samples after ultraviolet digestion, ascorbic acid for mixing with the mixture of the samples and the color reagent, a peristaltic pump for pumping the color reagent and ascorbic acid, and a heating reactor for the mixture thereof;

[0010] The detection module includes a flow cell for the final reaction product and a detector.

[0011] The integrated full-scenario adaptable total phosphorus rapid detection platform provided by this application integrates multiple modules such as raw water collection, sample digestion, sample injection and reaction, and detection, realizing the full-process automated operation from raw water collection to the output of the final detection result.

[0012] Furthermore, the entire process requires no manual intervention, greatly shortening the analysis time and reducing the operation difficulty. This makes the platform not only suitable for fine analysis in a laboratory environment, but also able to meet the rapid detection requirements in the field or industrial site, with significant advantages such as simple operation, fast detection speed, and high accuracy, providing a new solution for total phosphorus detection.

[0013] The automatic sampler can intelligently switch multiple sample tubes and online water samples, greatly improving the flexibility and efficiency of raw water treatment. The sample digestion module adopts a dual digestion method combining sulfuric acid and potassium persulfate, supplemented by a heating reactor and an ultraviolet digestion device, effectively improving the digestion efficiency and thoroughness, and ensuring the accuracy of subsequent detection results.

[0014] At the same time, between samples and between samples and reagents, there is no need to add bubbles, and there is no need to reach the physical mixing and chemical reaction equilibrium state to repeat the determination, realizing rapid and accurate analysis.

[0015] In some possible implementation manners, the raw water collection module further includes a sampling valve that can rotate multi-way and a sampling loop for the stable peristaltic pump to pump the raw water.

[0016] In some possible implementation manners, the raw water collection module further includes a carrier tank for pumping the carrier fluid by a peristaltic pump, and the carrier fluid in the carrier tank is pumped to the sampling valve and pushes the raw water in the sampling loop to the sample digestion module.

[0017] In some possible implementation manners, the sampling valve is provided with a waste liquid discharge port.

[0018] In some possible implementation manners, the number of the peristaltic pumps is 1, and the same peristaltic pump is used for the raw water collection module, the sample digestion module, and the sample injection and reaction module.

[0019] In some possible implementation manners, it further includes a surrounding reactor provided at the rear end after mixing with potassium persulfate and after mixing with the color reagent.

[0020] In some possible embodiments, the raw water collection module further includes a refrigeration device for controlling the temperature of the sample tube and / or the auto-sampler for raw water.

[0021] In a second aspect, the present application also provides a method for rapid total phosphorus detection and analysis using the integrated full-scenario adaptable total phosphorus rapid detection platform as described above. BRIEF DESCRIPTION OF THE DRAWINGS

[0022] Figure 1 is a schematic diagram of the integrated full-scenario adaptable total phosphorus rapid detection platform of the present application;

[0023] Figure 2 is a schematic diagram of the detection and analysis process flow of the integrated full-scenario adaptable total phosphorus rapid detection platform of the present application. DETAILED DESCRIPTION OF THE EMBODIMENTS

[0024] The following further details the features of the present application and other related features through examples for the understanding of those skilled in the same industry:

[0025] It should be noted that the terms "front", "rear", "left", "right", "upper" and "lower" used in the following description refer to the directions in the drawings, and the terms "bottom surface" and "top surface", "inner" and "outer" refer to the directions towards or away from the geometric center of a specific component respectively.

[0026] Furthermore, unless otherwise clearly specified and limited, the terms "install", "connect", "couple" should be understood in a broad sense. For example, it can be a fixed connection, a detachable connection, or an integral connection; it can be directly connected, or indirectly connected through an intermediate medium, and it can be the communication inside two components. For those of ordinary skill in the art, the specific meanings of the above terms in this case can be understood according to the specific situation.

[0027] The present application combines the advantages of flow injection analysis (FIA) technology and ammonium molybdate spectrophotometry to achieve high-sensitivity, rapid and accurate quantitative analysis of phosphorus elements. Further, first by combining flow injection analysis (FIA) technology and raw water sampling technology, on-line and off-line full-scenario adaptable raw water sampling can be realized, and at the same time, the production process from raw water to reaction samples is improved to achieve rapid detection and analysis in an automatic production line mode.

[0028] The main principle of ammonium molybdate spectrophotometry is that total phosphorus is converted into orthophosphate form under the action of potassium persulfate oxidant. Then, in an acidic medium, orthophosphate reacts with ammonium molybdate to form phosphomolybdic yellow, and then is reduced to phosphomolybdic blue with ascorbic acid, and the concentration of phosphorus is determined by measuring its absorbance at a specific wavelength. The following details it in combination with the overall automatic production line steps.

[0029] Please refer toFigure 1 Overall, the integrated full-scenario adaptable total phosphorus rapid detection platform of the present application includes a raw water collection module, a sample digestion module, an injection reaction module, and a detection module.

[0030] First of all, the raw water collection module includes an automatic sampler. The automatic sampler is mainly used to automatically extract raw water from multiple water sources or sample tubes and transport it to the next step of the detection platform. The transportation method can adopt a peristaltic pump. The peristaltic pump pushes the fluid by squeezing the hose instead of directly contacting the liquid, thus avoiding the pollution of the fluid and ensuring the accuracy of high-purity chemical analysis. And the flow rate can be easily changed by adjusting the rotation speed, which helps to maintain the consistency and reproducibility of experimental conditions.

[0031] Furthermore, the automatic sampler can adopt the form of a sampling needle to switch between multiple different sample tubes or online water samples. The switching method can be in a switchable form such as rotation or movement, which is a commonly used technical means in the industry and will not be specifically limited herein.

[0032] During the raw water sampling process, there are requirements for continuity and stability. Therefore, the raw water collection module of the present application also includes a multi-way rotatable collection valve and a sampling loop for stabilizing the raw water pumped by the peristaltic pump. The sampling loop can adopt a long-distance conveying pipeline. Through the long-distance sampling loop, continuous automatic injection of raw water can be achieved, and at the same time, it plays a buffering role in the entire raw water collection process, making the raw water collection smoother, adjusting the flow rate, ensuring the representativeness of the sample and enabling the sample to be accurately extracted and introduced. Further, it mainly achieves the uniformization and stability of the movement degree of the raw water through natural flow. Specifically, when implemented, the multi-way rotation characteristic of the collection valve can be utilized for switching.

[0033] After that, through the multi-way rotation of the collection valve, the carrier fluid is pumped and the sample in the sampling loop is pushed to the sample digestion module by the carrier fluid. This method helps to ensure the precise control of the sample volume and can avoid cross-contamination between samples. The carrier fluid is provided by an independent carrier fluid tank, and a peristaltic pump is provided between the carrier fluid tank and the collection valve. The carrier fluid can be ionized water or ultrapure water. After the sample in the sampling loop is pushed by the carrier fluid, the next round of sample collection can be continuously carried out.

[0034] In this way, the automatic sampler can intelligently switch between multiple sample tubes and online water samples, greatly improving the flexibility and efficiency of raw water treatment. At the same time, its sampling valve is provided with a waste liquid discharge port, and the remaining waste liquid in the raw water collection stage can be discharged to the waste liquid bottle through the channel of waste discharge 1.

[0035] As described above, the present application is a full-scenario adaptable detection platform that can switch raw water samples. Therefore, there will be environmental errors during the sampling process. To address this, the raw water collection module of the present application further includes a refrigeration device that can control the temperature of the sample tube and the raw water of the auto-sampler. Specifically, an in-built refrigerator can be used to adjust the temperature of the sample tube or the auto-sampler simultaneously or individually.

[0036] In some embodiments, after the above raw water collection is completed and pushed out by the carrier fluid, it passes through a pressure controller. At this time, the role of the pressure controller is to further homogenize the raw water sample. By making the pushed-out raw water sample go through a long-distance loop, its pressure becomes uniform, and the sample stably flows to the next step.

[0037] Since the present application is a full-scenario adaptable detection platform that can switch raw water samples, it is necessary to pre-treat the raw water in the early stage. The functional configuration of the pressure controller can be adjusted according to requirements, which is a commonly used technical means in the detection field and will not be elaborated in detail here.

[0038] After the raw water is pre-treated, it is input into the sample digestion module. For the sake of distinction during description, in the present application, the raw water to be collected is described as "sample" in the raw water stage. While in the back-end for reaction, "sample" is used to describe the digested water and reaction water in the digestion and reaction stages.

[0039] The sample digestion module includes sulfuric acid that is mixed with the raw water transported by the raw water collection module. Specifically, the sulfuric acid is pumped by a peristaltic pump and mixed with the raw water for the first time through a tee. The main function of the tee is to mix liquids, which is a commonly used fitting and will not be elaborated in detail here. The main purpose of mixing the raw water with sulfuric acid is to acidify the sample. During the total phosphorus determination process, acidification can prevent the phosphate in the sample from being adsorbed by other substances or undergoing chemical changes and helps with the subsequent digestion process.

[0040] The mixed solution after the first mixing passes through a heating reactor, which is mainly a device that provides a stable controlled environmental temperature. During this process, the role of the heating reactor is to help decompose the complex organic substances that may exist in the sample through heating in an acidic environment, converting them into soluble inorganic phosphates. This is crucial for ensuring that all forms of phosphorus (including organic phosphorus and inorganic phosphorus) can be detected. Specifically, heating can accelerate the speed of chemical reactions, enabling phosphorus compounds to be converted into orthophosphate form faster, thereby improving the efficiency of the entire analysis process.

[0041] Further, in order to ensure that all phosphorus elements can exist in the form of orthophosphate, the mixed solution transported to the heating reactor is secondarily mixed with potassium persulfate through a three-way pipe. Potassium persulfate is a strong oxidant that can effectively oxidize phosphorus in various forms completely into orthophosphate, facilitating the subsequent determination by ammonium molybdate spectrophotometry. The potassium persulfate is transported through a peristaltic pump to be secondarily mixed with the mixed solution, and the mixed solution after the secondary mixing is subjected to ultraviolet digestion. Ultraviolet irradiation can enhance the oxidation ability of potassium persulfate because ultraviolet light can stimulate potassium persulfate to generate stronger oxidizing species, such as hydroxyl radicals, etc. These active species can more effectively destroy complex organic structures to ensure the complete oxidation of phosphorus. In addition, ultraviolet disinfection also helps to degrade interfering substances that may exist in the sample, such as certain organic substances or other non-target components, reducing their influence on the phosphorus determination result. In this way, the sample preparation process for the reaction can be completed and transported to the injection reaction module.

[0042] The injection reaction module includes a color reagent that is thirdly mixed with the sample after ultraviolet digestion, ascorbic acid that is fourthly mixed with the sample after the third mixing, a peristaltic pump for pumping the color reagent and ascorbic acid, and a heating reactor for heating and reacting the mixed solution after the fourth mixing.

[0043] Specifically, after the sample and the color reagent are thirdly mixed through a three-way pipe, the mixed solution passes through the surrounding reactor. At this stage, the main function of the surrounding reactor is to provide a space for sufficient mixing and reaction to ensure that the color reagent (such as ammonium molybdate) can fully react with the orthophosphate in the sample to form phosphomolybdic heteropolyacid. Further, after the third mixed solution is fourthly mixed with ascorbic acid through a three-way pipe, it passes through the heating reactor to accelerate the conversion process of phosphomolybdic heteropolyacid into phosphomolybdenum blue complex.

[0044] At this time, the color reagent uses ammonium molybdate solution. Ammonium molybdate reacts with the orthophosphate in the sample to form phosphomolybdic heteropolyacid, and is further converted into blue phosphomolybdenum blue complex under the action of ascorbic acid. Ascorbic acid, that is, vitamin C, acts as a reducing agent to reduce phosphomolybdic heteropolyacid to phosphomolybdenum blue complex. The absorbance of this complex at a specific wavelength can be used for quantitative analysis of the phosphorus content. Then it enters the detection module, and the detection module includes a flow cell for the final reaction product and a detector for quantitatively analyzing the phosphorus content. In some embodiments, the detector is connected to a data processing workstation to automatically analyze the data.

[0045] In this way, the integrated full-scenario adaptable total phosphorus rapid detection platform provided by this application integrates multiple modules such as raw water collection, sample digestion, injection reaction, and detection into one, realizing the full-process automated operation from raw water collection to the output of the final detection result.

[0046] Furthermore, the entire process requires no manual intervention, greatly shortening the analysis time and reducing the operation difficulty. This makes the platform not only suitable for fine analysis in a laboratory environment but also capable of meeting the rapid detection needs in the field or industrial sites, with significant advantages such as easy operation, fast detection speed, and high accuracy, providing a new solution for total phosphorus detection.

[0047] Meanwhile, no bubbles need to be added between samples and between samples and reagents, enabling rapid and accurate analysis.

[0048] In the above embodiments, peristaltic pumps are used to transport liquids in the raw water sampling module, sample digestion module, and sample injection reaction module. At this time, it is preferred to use 1 peristaltic pump, which reduces the number of devices, makes the entire detection process more compact and efficient, also reduces complexity, and is convenient for installation and maintenance. At the same time, such an integrated design also reduces the operation errors that may be introduced by using multiple pumps, further improving the reliability and consistency of the measurement results.

[0049] A method for rapid total phosphorus detection and analysis using the integrated full-scenario adaptable total phosphorus rapid detection platform as described above is as follows.

[0050] Step S1: The auto-sampler samples the raw water sample and transports it to the sampling valve through a peristaltic pump;

[0051] Step S2: Control through the sampling valve to make the raw water sample pass through the sampling loop and push the sample to the sample digestion module through the carrier flow;

[0052] Step S3: After the sample is pushed, it is first mixed with the pumped sulfuric acid through a tee and then transported to the heating reactor 1;

[0053] Step S4: The mixed solution after the heating reaction is mixed with the pumped potassium persulfate for the second time and then transported to the ultraviolet digestion;

[0054] Step S5: The mixed solution after the ultraviolet digestion is mixed with the pumped color reagent for the third time and then mixed with the pumped ascorbic acid for the fourth time and then transported to the heating reactor 2;

[0055] Step S6: The mixed solution after the reaction in the heating reactor 2 is transported to the flow cell and detected by the detector.

[0056] In this way, fully automatic rapid total phosphorus detection can be completed. For automatic sampling, during the execution of step S1 of this application, it may further include step S11: the step of automatically switching between multiple sample tubes or online water samples by the auto-sampler.

[0057] For the treatment of the residual waste liquid of the sampling valve during the switching process, it can be completed through a waste liquid bottle communicated with the sampling valve. Before performing step S1, step S12 is executed: drain the waste liquid of the waste sampling valve into the waste liquid bottle.

[0058] As described above, the present application protects an integrated full-scenario adaptable total phosphorus rapid detection platform and analysis method. All technical solutions identical or similar to this case should be shown to fall within the protection scope of this case.

Claims

1. An integrated full-scenario adaptive total phosphorus rapid detection platform, characterized by: It includes raw water collection module, sample digestion module, injection reaction module and detection module; The raw water collection module includes an automatic sampler and a peristaltic pump that can automatically switch between multiple sample tubes and / or collect raw water between online water samples; The sample digestion module includes sulfuric acid mixed with the sample delivered by the raw water collection module through a tee, a peristaltic pump for pumping the sulfuric acid, and a heating reactor for the mixed solution, potassium persulfate mixed with the mixed solution delivered by the heating reactor, a peristaltic pump for pumping the potassium persulfate, and an ultraviolet digestion device for the mixed solution; The injection reaction module includes a color developer mixed with the sample after UV digestion, ascorbic acid mixed with the mixed solution of the sample and the color developer, a peristaltic pump for pumping the color developer and the ascorbic acid, and a heating reactor for the mixed solution; The detection module includes a flow cell for the final reaction product and a detector.

2. The integrated full-scenario adaptive total phosphorus rapid detection platform according to claim 1, characterized in that: The raw water collection module also includes a multi-rotatable sampling valve and a sampling ring for stably pumping raw water with a peristaltic pump.

3. The integrated full-scenario adaptive total phosphorus rapid detection platform as described in claim 2 is characterized in that: The raw water collection module also includes a flow tank for pumping a flow through a peristaltic pump. The flow in the flow tank is pumped to a sampling valve and pushes the raw water in the sampling loop to a sample digestion module.

4. The integrated full-scenario adaptive total phosphorus rapid detection platform as described in claim 2 is characterized in that: The sampling valve is provided with a waste liquid discharge port.

5. The integrated full-scenario adaptive total phosphorus rapid detection platform according to claim 1, characterized in that: The number of the peristaltic pump is 1, and the raw water collection module, the sample digestion module, and the sample injection reaction module use the same peristaltic pump.

6. The integrated full-scenario adaptive total phosphorus rapid detection platform according to claim 1, characterized in that: The invention also comprises a surrounding reactor arranged at the rear end after mixing with potassium persulfate and mixing with a developer.

7. The integrated full-scenario adaptive total phosphorus rapid detection platform according to claim 1, characterized in that: The raw water collection module also includes a refrigeration device capable of controlling the raw water temperature of the sample tube and / or the automatic sampler.

8. An integrated full-scenario adaptive total phosphorus rapid detection and analysis method, characterized in that: The integrated full-scenario adaptive total phosphorus rapid detection platform as claimed in any one of claims 1 to 7 is used, and the steps include: Step S1: the automatic sampler samples the raw water sample and delivers it to the sampling valve through the peristaltic pump; Step S2: controlling the raw water sample to pass through the sampling ring through the sampling valve, and pushing the sample to the sample digestion module through the carrier current; Step S3: After the sample is pushed, it is mixed with the pumped sulfuric acid through a three-way connection for the first time and then transported to the heating reactor 1; Step S4: the mixed solution after the heating reaction is mixed with the pumped potassium persulfate for a second time and then transported to ultraviolet digestion; Step S5: the mixed solution after UV digestion is mixed with the pumped color developer for the third time, and then mixed with the pumped ascorbic acid for the fourth time and then transported to the heating reactor 2; Step S6: the mixed solution after the reaction in the heating reactor 2 is transported to the circulation pool and detected by the detector.

9. The integrated full-scenario adaptive total phosphorus rapid detection and analysis method according to claim 8, characterized in that: The execution process of step S1 may also include step S11: the step of automatically switching the automatic sample injector between multiple sample tubes or online water samples.

10. The integrated full-scenario adaptive total phosphorus rapid detection and analysis method according to claim 8, characterized in that: Before executing step S1, execute step S12: discharge the waste liquid of the waste sampling valve into the waste liquid bottle.

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