High-concentration matrix eliminating device

By employing ammonium acetate complexation and enrichment column adsorption, the problem of detecting heavy metal ions in high-concentration matrices was solved, thereby improving detection sensitivity and accuracy, resolving the accuracy issue in high-concentration matrices, and achieving efficient heavy metal ion detection.

CN223637202UActive Publication Date: 2025-12-05QINGDAO SHENGHAN CHROMATOGRAPH TECH CO LTD
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Patent Information

Application Number
CN202422945927.4
Authority / Receiving Office
CN · China
Patent Type
Utility models(China)
Current Assignee / Owner
Filing Date
2024-12-02
Publication Date
2025-12-05
Estimated Expiration
2034-12-02

AI Technical Summary

Technical Problem

In high-concentration matrices, target analytes such as heavy metal ions are difficult to detect accurately. Existing technologies are difficult to use and have low accuracy, especially in seawater or industrial wastewater, where the matrix effect significantly interferes with detection.

Method used

A high-concentration matrix elimination device was designed. It forms a complex with heavy metal ions using ammonium acetate and selectively adsorbs them using an enrichment column. Combined with nitric acid desorption, it achieves the enrichment and cleaning of the target analyte. The fluid control system consists of components such as an autosampler, reagent bottles, a plunger pump, a six-way valve, and an enrichment column.

Benefits of technology

It significantly improves the detection sensitivity and accuracy of target analytes, effectively removes interference from high-concentration matrix components, and enhances the reliability and precision of detection.

✦ Generated by Eureka AI based on patent content.

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Abstract

The utility model relates to the field of environmental monitoring and analytical chemistry, in particular to a high-concentration matrix eliminating device which comprises an automatic sample injector, a first reagent bottle for storing nitric acid, a second reagent bottle for storing ammonium acetate, a third reagent bottle for storing ultrapure water, a three-way pipe, an enriching column, a six-way valve and an automatic fraction collector, the first reagent bottle, the second reagent bottle and the third reagent bottle are sequentially connected with a first connector through pipelines, the first connector is used for switching and selecting passages, the outlet end of the first connector is connected with a first plunger pump through a selector valve, and six connecting points are arranged in the six-way valve. A first connecting point of the six-way valve is connected with the first plunger pump, the three-way pipe is provided with three connecting ends, a second connecting point of the six-way valve is connected with a first connecting end of the three-way pipe, and a sample injection needle of the automatic sample injector is connected with the second connector through a pipeline. The utility model solves the problem that a target analyte exists in a high-concentration matrix and is difficult to detect.
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Description

TECHNICAL FIELD

[0001] The utility model relates to environmental monitoring and analytical chemistry field especially, relate to a high concentration matrix elimination device. BACKGROUND

[0002] In modern environmental monitoring and industrial production process, accurately determining the heavy metal content in water is crucial because it is directly related to human health and environmental protection.

[0003] In the prior art, detecting heavy metals in seawater usually requires a series of pretreatment steps to ensure that these trace or even trace level heavy metal ions can be accurately detected. One commonly used method is to use a quantitative ring for detection. The disadvantage of this method is that when the heavy metal concentration in the sample is very low, the detection difficulty will increase. Seawater contains a large amount of salts and other compounds, which may interfere with the detection of heavy metal ions. Especially in the case of low concentration, the matrix effect is more obvious, further reducing the accuracy of detection.

[0004] High concentration matrix elimination refers to a process in analytical chemistry to remove or reduce the interference of high concentration matrix components in the sample on the detection of target analytes in order to improve analysis accuracy and accuracy. In practical applications, when the target analyte (such as heavy metal ions) exists in a high concentration matrix (such as sodium chloride in seawater or industrial wastewater), detection becomes complex and difficult because the signal of the target substance is easily masked or interfered by the high concentration matrix component, making it difficult to be accurately detected. The present utility model is designed to solve the above technical problems, and a high concentration matrix elimination device is designed. UTILITY MODEL CONTENT

[0005] The utility model provides a kind of high concentration matrix elimination device, to solve the problem that target analyte exists in high concentration matrix is difficult to detect, its technical scheme is as follows:

[0006] A kind of high concentration matrix elimination device, including automatic sampler, first reagent bottle for storing nitric acid, second reagent bottle for storing ammonium acetate, third reagent bottle for storing ultrapure water, tee, enrichment column, six-way valve and automatic fraction collector;

[0007] The first reagent bottle, the second reagent bottle and the third reagent bottle are sequentially connected with a first connector through pipelines, the first connector is used for switching selection of a channel, outlet ends of the first connector are all connected with a first plunger pump through a selection valve, six connection points are arranged in the six-way valve, a first connection point of the six-way valve is connected with the first plunger pump, the three-way pipe is provided with three connection ends, a second connection point of the six-way valve is connected with a first connection end of the three-way pipe, a sampling needle of the automatic sampler is connected with a second connector through a pipeline, the second connector is used for switching selection of a channel, the second connector is connected with a second plunger pump, the second plunger pump is connected with a second connection end of the three-way pipe, one end of the enrichment column is connected with a third connection end of the three-way pipe, and the other end is connected with a flow-out device; and the flow-out device is connected with an automatic fraction collector.

[0008] On the basis of the above technical scheme, the third connection point and the fourth connection point of the six-way valve are respectively communicated with two ends of the guard column.

[0009] Further, the first plunger pump and the second plunger pump are respectively connected with a first pressure sensor and a second pressure sensor.

[0010] Preferably, the flow-out device is further connected with a waste collector.

[0011] Beneficial effects

[0012] Compared with the prior art, the beneficial effects of the present application are as follows: on the one hand, the complex of ammonium acetate and heavy metal ions in the sample can be chelated on the enrichment column, which significantly improves the detection sensitivity of the target analyte, especially when dealing with samples containing high-concentration matrix components; on the other hand, by accurately controlling the delivery and selection of the fluid, the interference of high-concentration matrix components in the sample on the detection of the target analyte is effectively removed or reduced, and the accuracy and reliability of the detection are improved. BRIEF DESCRIPTION OF DRAWINGS

[0013] In order to more clearly illustrate the technical scheme in the embodiments of the present application or the prior art, the drawings needed in the following embodiment or prior art description will be briefly introduced. Obviously, the drawings in the following description are only one embodiment of the present application, and those skilled in the art can obtain other embodiment drawings according to the provided drawings without creating any creative labor.

[0014] Figure 1 : the structure diagram of the present application;

[0015] Figure 2 : the first enlarged view of the local part of the present application;

[0016] Figure 3The second partial enlarged view. DETAILED DESCRIPTION

[0017] The utility model will be further described below in combination with the drawings and examples:

[0018] The embodiments of the utility model will be described in detail below, and the examples of the embodiments are shown in the drawings, wherein the same or similar reference signs represent the same or similar elements or elements with the same or similar functions throughout. The embodiments described below by referring to the drawings are exemplary and are only used to explain the utility model, and cannot be understood as a limitation on the utility model.

[0019] In the description of the utility model, it should be explained that, unless otherwise explicitly specified and limited, the terms "mounting", "connection", "connection" should be understood broadly, for example, it can be fixed connection, or detachable connection, or integrally connected, it can be directly connected, or indirectly connected through intermediate medium. For ordinary skilled in the art, the specific meaning of the above terms in the utility model can be understood according to specific circumstances.

[0020] In the description of the utility model, it should be understood that the terms "up", "down", "front", "back", "left", "right", "vertical", "horizontal", "top", "bottom", "inside", "outside" and the like indicate the orientation or positional relationship shown in the drawings, and are only used to facilitate the description of the utility model and simplify the description, and are not indicative or implied that the device or element referred to must have a particular orientation, a particular orientation and operation, therefore, it cannot be understood as a limitation on the utility model.

[0021] As shown in FIG. 1 to Figure 3 A high-concentration matrix elimination device: comprising an automatic sampler 1, a first reagent bottle 2 for storing nitric acid, a second reagent bottle 3 for storing ammonium acetate, a third reagent bottle 4 for storing ultrapure water, a tee joint 64, an enrichment column 65, a six-way valve 66 and an automatic fraction collector 7.

[0022] The first reagent bottle 2, the second reagent bottle 3 and the third reagent bottle 4 are connected in sequence by a pipeline to the first connector 51, the first connector 51 is used for switching selection of the passage, the outlet end of the first connector 51 is connected to the first plunger pump 53 through a selection valve 52, six connection points are arranged in the six-way valve 66, the first connection point of the six-way valve 66 is connected to the first plunger pump 53, the three-way pipe 64 is provided with three connection ends, the second connection point of the six-way valve 66 is connected to the first connection end of the three-way pipe 64, the sampling needle of the automatic sampler 1 is connected to the second connector 61 through a pipeline, the second connector 61 is used for switching selection of the passage, the second connector 61 is connected to the second plunger pump 62, the second plunger pump 62 is connected to the second connection end of the three-way pipe 64, one end of the enrichment column 65 is connected to the third connection end of the three-way pipe 64, and the other end is connected to the outflow device 68; the outflow device 68 is connected to the automatic fraction collector 7

[0023] In the process of high-concentration matrix elimination, ammonium acetate is added to the sample to promote the formation of a complex of heavy metal ions in the sample and ammonium acetate, so that selective adsorption can be achieved on the subsequent enrichment column. As a buffer solution, ammonium acetate can maintain the pH value of the solution in a relatively stable range, which is conducive to the complexation of certain metal ions. Ammonium acetate can chelate heavy metal ions in the sample on the enrichment column.

[0024] The first connector 51 is used for connecting and selecting the first reagent bottle 2, the second reagent bottle 3 and the third reagent bottle 4 for subsequent configuration, and the selection valve 52 is used for controlling the inflow of different reagents. The selection valve 52 can switch the internal channel through an external control signal, and by switching the position of the selection valve 52, it can be determined which reagent bottle solution is transported to the subsequent assembly. The first plunger pump 53 is used for accurately controlling the delivery amount of the fluid. By adjusting the stroke of the plunger pump, the volume of the delivered fluid can be controlled. The first plunger pump 53 is provided with a first pressure sensor 54, which is used to monitor the pressure condition of the first plunger pump 53 during operation, to ensure the stability and safety of fluid delivery. The selected solution is transported to the six-way valve 66 through the subsequent pipeline connection.

[0025] In use, the automatic sampler 1 is used to automatically feed the sample to be tested into the system. The sample is sucked in through the sampling needle and transported to the second connector 61 through the pipeline. The sample is transported to the second plunger pump 62 through the second connector 61, and the second plunger pump 62 is responsible for controlling the speed and amount of sample delivery. The second plunger pump 62 is provided with a second pressure sensor 63 for monitoring the working state of the pump. The sample enters the three-way pipe 64 from the second connection end of the three-way pipe 64 through the second plunger pump 62, and is mixed with ammonium acetate from the ammonium acetate bottle 3 at this point.

[0026] Ammonium acetate is delivered from the second reagent bottle 3 through the first connector 51 and the selection valve 52 to the six-way valve 66 by the first plunger pump 53. Ammonium acetate enters the six-way valve 66 from the first connection point of the six-way valve 66, and the third and fourth connection points of the six-way valve 66 are respectively connected to the two ends of the guard column 67, ensuring that only pure ammonium acetate solution enters the system. Ammonium acetate enters the three-way tube 64 from the second connection point of the six-way valve 66 and mixes with the sample.

[0027] In the three-way tube 64, heavy metal ions in the sample form a complex with ammonium acetate, and ammonium acetate acts as a buffer solution to maintain the pH value within a stable range, which is conducive to the complexation of metal ions. After complexation, the heavy metal ions enter the enrichment column 65 along with the sample, and are selectively adsorbed on the enrichment column 65. The stationary phase on the enrichment column 65 can specifically chelate with heavy metal ions, achieving enrichment of target ions.

[0028] Nitric acid acts as a leaching solution to promote the desorption of adsorbed heavy metal ions from the enrichment column 65, facilitating subsequent quantitative analysis. Nitric acid is stored in the first reagent bottle 2. When the leaching operation is required, the nitric acid solution is delivered from the first reagent bottle 2 through the pipeline, the first connector 51, the selection valve 52, and the first plunger pump 53 to the six-way valve 66. The six-way valve 66 is a valve that allows fluid to enter from different inlets and flow out through different outlets, thereby realizing multiple fluid path configurations. It allows the nitric acid solution to flow to the three-way tube 64. The six-way valve 66 is provided with a guard column 67 to prevent impurities from entering the enrichment column 65. The nitric acid solution enters the three-way tube 64 through the six-way valve 66. The nitric acid solution enters the enrichment column 65 through the three-way tube 64. In the enrichment column 65, nitric acid as a strong acid can effectively desorb heavy metal ions that have been adsorbed on the stationary phase, thereby releasing them from the enrichment column. At the same time, nitric acid also plays a role in cleaning the enrichment column, removing possible residual impurities, and ensuring that the enrichment column is in a clean state.

[0029] The desorbed heavy metal ions flow out with the nitric acid solution through the effluent 68. The effluent 68 is connected to the automatic fraction collector 7 for collecting the solution containing the desorbed target metal ions. The desorbed heavy metal ion solution is collected by the automatic fraction collector 7 for subsequent analysis, such as inductively coupled plasma mass spectrometry. ICPMS is used to detect and quantify metals and some non-metal elements in the sample, has a wide dynamic range and the ability to analyze multiple elements simultaneously, is suitable for trace element analysis and isotope ratio determination in multiple fields, can handle complex matrix samples and provide accurate and reliable detection results in a short time. The automatic fraction collector 7 can collect different fractions at set time or volume intervals, thereby facilitating further processing and analysis.

[0030] In the process of high concentration matrix elimination, ammonium acetate is added to promote the formation of complex of heavy metal ions in the sample, so that these ions can be selectively adsorbed on the enrichment column. The ultrapure water has two functions in this process: one is to help push the reaction solution through the enrichment column 65, and the other is to clean the pipeline to ensure that there is no residual material to interfere with subsequent analysis. The ultrapure water can be added in the following two steps:

[0031] After adding the sample: The addition of ultrapure water can help adjust the total volume of the reaction system, ensure the consistency of the reaction conditions, and help push the reaction solution through the enrichment column 65 later. After the addition of ultrapure water, the volume of the reaction solution increases, which helps to push the reaction solution through the flow path of the system. Especially adding ultrapure water before the enrichment column 65 can ensure that the reaction solution is evenly distributed and has enough power to pass through the enrichment column.

[0032] After adding ammonium acetate: The addition of ultrapure water at this time can help push the sample that has reacted with ammonium acetate to form a complex to the enrichment column 65, ensuring that all the reaction solution can smoothly pass through and be adsorbed by the enrichment column. After the sample treatment is completed, the addition of ultrapure water can help clean the pipeline and other components in the reaction path. The ultrapure water can flush away the residual sample or reagent, ensuring that subsequent samples are not cross-contaminated. The effluent 68 is also connected to the waste collector. After flushing, it can flow to the waste collector through the effluent 68.

[0033] It should be noted that the autosampler 1, connector, plunger pump, selection valve 52, six-way valve 66, pressure sensor and automatic fraction collector 7 in the embodiment are all general standard parts or components known to those skilled in the art, and their structure and principle can be known by those skilled in the art through technical manuals or through conventional experimental methods.

[0034] The utility model has been described above by way of example, but the utility model is not limited to the above specific embodiments, and any modification or modification based on the utility model falls within the scope of the utility model claimed.

Claims

1. A high concentration matrix elimination device characterized by: The device comprises an automatic sample injector (1), a first reagent bottle (2) for storing nitric acid, a second reagent bottle (3) for storing ammonium acetate, a third reagent bottle (4) for storing ultrapure water, a three-way pipe (64), an enrichment column (65), a six-way valve (66) and an automatic fraction collector (7). The first reagent bottle (2), the second reagent bottle (3) and the third reagent bottle (4) are sequentially connected with a first connector (51) through pipelines, the first connector (51) is used for switching selection of a passage, outlet ends of the first connector (51) are connected with a first plunger pump (53) through a selection valve (52), six connection points are arranged in the six-way valve (66), a first connection point of the six-way valve (66) is connected with the first plunger pump (53), the three-way pipe (64) is provided with three connection ends, a second connection point of the six-way valve (66) is connected with a first connection end of the three-way pipe (64), a sample injection needle of the automatic sample injector (1) is connected with a second connector (61) through a pipeline, the second connector (61) is used for switching selection of a passage, the second connector (61) is connected with a second plunger pump (62), the second plunger pump (62) is connected with a second connection end of the three-way pipe (64), one end of the enrichment column (65) is connected with a third connection end of the three-way pipe (64), and the other end is connected with an effluent device (68); the effluent device (68) is connected with the automatic fraction collector (7).

2. The high concentration matrix elimination device according to claim 1, characterized by: The third connection point and the fourth connection point of the six-way valve (66) are respectively communicated with two ends of a guard column (67).

3. The high concentration matrix elimination device of claim 1, wherein: The first plunger pump (53) and the second plunger pump (62) are respectively connected with a first pressure sensor (54) and a second pressure sensor (63).

4. The high concentration matrix elimination device of claim 1, wherein: The effluent device (68) is further connected with a waste collector.