A device for removing interference for ion chromatographic determination of anions in high-salt seawater

Abstract

The application discloses a device for removing interference for ion chromatography determination of anions in high-salt seawater, and relates to the technical field of instrumental analysis.The device comprises a working column group, the working column group is connected with a chromatograph through a conveying pipe, the working column group is at least two, upper ends of the working column group are connected with first pipe bodies, and electric control valves are arranged at the connecting positions, and the working column group comprises a main pretreatment column and an auxiliary pretreatment column which are connected in series.The device solves the problems of signal distortion of chromatographic detection, shortening of the service life of a chromatographic column and difficulty in accurate determination of low-concentration target ions caused by interfering ions in high-salt seawater in the prior art, and has the advantages of simple operation, low cost, high automation degree and good compatibility.

Description

Technical Field

[0001] This invention relates to the field of instrumental analysis technology, specifically to an interference removal device for the determination of anions in high-salinity seawater using ion chromatography. Background Technology

[0002] Ion chromatography, a type of high-performance liquid chromatography, is widely used in the analysis of anions and cations. It achieves ion separation through the principle of ion exchange and is detected by detectors such as conductivity and ultraviolet light. It offers advantages such as fast analysis speed, good selectivity, and the ability to simultaneously determine multiple components. However, determining anions in high-salinity seawater presents numerous challenges.

[0003] Seawater is considered a liquid mineral resource, with an average salinity of 35‰. Each cubic kilometer of seawater contains approximately 35.7 million tons of minerals, and over 80% of the more than 100 known elements can be found in it. The main salts in seawater include a large amount of Cl. - and SO4 2⁻ In cases where high concentrations of interfering ions are present, direct injection for ion chromatography analysis can saturate the conductivity detector, causing the chromatographic column to malfunction due to overload. This severely masks the signals of low-concentration target anions (such as nitrates and nitrites), making detection difficult.

[0004] Traditional methods have significant limitations. While dilution is simple, it drastically reduces detection sensitivity, leading to higher detection limits and failing to meet the requirements for detecting trace anions in seawater. Solid-phase extraction requires extensive manual operation, is cumbersome, and resin regeneration is difficult, hindering large-scale applications. Online matrix removal technology is highly dependent on specific instruments, costly, and lacks compatibility with different sample types, limiting its practical application. Existing technologies offer several solutions to these problems, such as DE102014226481B3, which implements a multi-channel valve unit in the sample metering and separation column switching device of a gas chromatograph. Another example is JP07134120A, which discloses a method and apparatus for ion neutralization. This neutralization device concentrates metal ions within the solution column, resulting in neutralization, and then drains the liquid from the column into a second neutralization device. However, the effectiveness of these devices in treating Cl- in seawater remains a challenge. - and SO4 2⁻ There is still room for improvement in aspects such as these elements. Summary of the Invention

[0005] The purpose of this invention is to provide an interference removal device for the determination of anions in high-salinity seawater by ion chromatography, which solves the problems of chromatographic detection signal distortion, shortened column life, and difficulty in accurately determining low-concentration target ions caused by interfering ions in high-salinity seawater in the prior art. It has the advantages of simple operation, low cost, high degree of automation, and good compatibility.

[0006] To solve the above-mentioned technical problems, the present invention specifically provides the following technical solution: an interference removal device for the determination of anions in high-salt seawater by ion chromatography, comprising a working column group, the working column group being connected to a chromatograph via a delivery pipe, the working column group having at least two components, the upper ends of the working column group being connected to a first tube body, and an electrically controlled valve being provided at the connection point, the working column group comprising a main pretreatment column and a secondary pretreatment column connected vertically.

[0007] This invention reduces the concentration of interfering elements in seawater by combining a main pretreatment column and a secondary pretreatment column in series, meeting the requirements for the detection of trace anions in ion chromatography and solving the problem of high-salt matrix masking the chromatographic signal. Furthermore, this invention uses a dual working column group that can be dynamically switched according to usage requirements. That is, when one working column group is performing ion removal, the other working column group simultaneously completes backwashing, regeneration, and activation, avoiding the need to shut down the traditional single-column system.

[0008] According to one embodiment of the present invention, both the main pretreatment column and the sub-pretreatment column are filled with resin, and the cationic or anionic raw materials loaded in the main pretreatment column and the sub-pretreatment column are different. Different resins have different loaded raw materials, enabling separate treatment of Cl... - and SO4 2⁻ Elements and cations work together to prevent overloading of a single resin column.

[0009] According to one embodiment of the present invention, there are at least two secondary pretreatment columns, and both primary pretreatment columns are filled with functionalized Ag with a particle size of 40 μm. + Supported sulfonic acid ion exchange resin, at least one secondary pretreatment column contains functionalized Ba with a particle size of 40 μm. 2+ A cation-supported resin column, with at least one secondary pretreatment column containing functionalized Na particles with a particle size of 40 μm. + A cation exchange resin-supported column is used. At least two secondary pretreatment columns are provided, forming a series flow with the main pretreatment column to achieve Cl... - and SO4 2⁻ It also features stepwise removal of cations, avoiding the efficiency drop caused by loading too many types of ions onto a single resin column; at the same time, the modular resin column design allows for independent replacement of failed resins, reducing maintenance costs, and the column sequence can be flexibly adjusted according to seawater salinity fluctuations to adapt to different detection scenarios.

[0010] According to one embodiment of the present invention, a third tube is connected to one side of both the main pretreatment column and the sub-pretreatment column. The third tube is connected to the side of both the main pretreatment column and the sub-pretreatment column. When a pressure sensor or conductivity sensor detects a decrease in resin column performance, a high-pressure chromatography pump can directionally push backwash solution into a single column through the third tube to precisely dissolve the AgCl precipitate in the main pretreatment column or the BaSO4 precipitate in the sub-pretreatment column, avoiding interference of the regeneration solution with other columns and improving regeneration efficiency.

[0011] According to one embodiment of the present invention, an auxiliary component is built into the end of the main pretreatment column near the third tube. The auxiliary component includes two spaced-apart first filter plates. A first support rod is fixedly connected to the bottom surface of the first filter plate, and a second support rod is spaced apart on the side of the first support rod and perpendicular to its axis. The two spaced-apart first filter plates form a filter jacket, which can intercept particulate impurities in seawater, such as silt and biological debris, improve the rejection rate of solid particles ≥40μm, and prevent impurities from clogging the resin pores. At the same time, the porous structure of the filter plate allows the sample flow to be uniformly dispersed into the resin layer, reducing local processing blind spots caused by fluid short circuits. Furthermore, the first support rod is vertically fixed to the bottom surface of the filter plate, and the second support rod is radially spaced and perpendicular to the first support rod, forming a support frame, which improves the load-bearing capacity of the filter plate, can withstand the fluid impact when pushed by the high-pressure chromatography pump, and prevents the filter plate from deforming and causing resin leakage.

[0012] According to one embodiment of the present invention, a first leaf plate and a second leaf plate arranged in a ring are provided between two first filter plates. The first leaf plate is connected to the surface of one of the first filter plates, and the second leaf plate is connected to the surface of the other first filter plate. The first leaf plate and the second leaf plate are connected by a second ring. There are at least three first leaf plates, which are arranged at intervals around the axis of the first filter plates. Adjacent first leaf plates are fixed by a first connecting ring. There are at least three second leaf plates, which are arranged at intervals around the axis of the first filter plates. Adjacent second leaf plates are fixed by a third connecting ring. The first connecting ring, the second connecting ring, and the third connecting ring all have through holes in their middle portions.

[0013] At least three first blades are arranged in a ring on one side of the first filter plate and connected to at least three second blades via second rings, forming a multi-layered radial flow channel. When the sample flows through, it is cut into multiple fine streams by the blades, increasing the contact area between the fluid and the resin. Adjacent first blades are fixed by first connecting rings, and adjacent second blades are fixed by third connecting rings, forming a stable flow channel framework. This improves the uniformity of fluid distribution along the column's radial direction, avoiding the situation where the flow velocity is high at the center and slow at the edges in traditional columns. This ensures a balanced resin utilization rate throughout the column. Furthermore, the through holes in the middle of the first, second, and third connecting rings allow the fluid to pass axially, increasing the overall pressure drop compared to a bladeless structure. This maintains a stable flow rate even when pushed by a high-pressure chromatography pump, avoiding the risk of system overload due to excessive pressure drop.

[0014] According to one embodiment of the present invention, the discharge end of the working column assembly is provided with a collection container. One end of the collection container is connected to the sub-pretreatment column, and the other end is connected to the chromatograph injection end through a delivery tube. The direct connection between one end of the collection container and the discharge end of the sub-pretreatment column, and the connection between the other end and the chromatograph injection end through a delivery tube, avoids the contamination risk caused by traditional manual sample transfer and shortens the detection process time.

[0015] According to one embodiment of the present invention, a high-pressure chromatography pump is connected to the first tube. The high-pressure chromatography pump delivers seawater samples to the working column assembly through the first tube. The stable pressure provided drives the high-salt, high-viscosity seawater through the resin column quickly, shortening the pretreatment time for a single sample.

[0016] According to one embodiment of the present invention, the working column assembly is mounted on a second frame, the second frame having a spare column communicating with the first tube, and the bottom of the second frame being connected to the first frame, on which the chromatograph is mounted. The second frame and the first frame are connected at the bottom to form a stable base, preventing loosening of the tubing or displacement of the resin column due to vibration, and ensuring the stability of fluid transmission.

[0017] According to one embodiment of the present invention, both the main pretreatment column and the auxiliary pretreatment column are equipped with pressure sensors and conductivity sensors. After the resin column has been used for a long time, the performance degradation of the resin column is judged by the feedback of the monitoring values ​​of the pressure and conductivity sensors. The regeneration system is then triggered and started. A high-pressure chromatography pump is used to push backwash solution to dissolve the precipitate in the resin column, followed by flushing with pure water, and then regeneration solution is pushed to activate and regenerate the resin column.

[0018] Compared with the prior art, the beneficial effects of the present invention are as follows: The present invention can reduce the concentration of interfering elements in seawater by combining the main pretreatment column and the sub-pretreatment column in series, thus meeting the requirements of ion chromatography for the detection of trace anions. Furthermore, the present invention adopts a dual working column group that can be dynamically switched according to the usage requirements. That is, when one working column group is performing ion removal, the other working column group simultaneously completes backwashing, regeneration and activation, avoiding the need for shutdown of traditional single column systems. The present invention can solve the problems of chromatographic detection signal distortion, shortened column life and difficulty in accurately measuring low-concentration target ions caused by interfering ions in high-salinity seawater in the prior art. It has the advantages of simple operation, low cost, high degree of automation and good compatibility. Attached Figure Description

[0019] To more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly introduced below. Obviously, the drawings described below are merely exemplary, and those skilled in the art can derive other embodiments based on the provided drawings without creative effort.

[0020] Figure 1 This is a schematic diagram of an interference removal device for the determination of anions in high-salt seawater using ion chromatography according to the present invention.

[0021] Figure 2 This is a partial schematic diagram of an interference removal device for ion chromatography determination of anions in high-salt seawater according to the present invention.

[0022] Figure 3 This is a schematic diagram of the working column assembly scheme of the present invention;

[0023] Figure 4 This is a schematic diagram of the internal structure of the main pretreatment column of the present invention;

[0024] Figure 5 This is a schematic diagram of the auxiliary component scheme of the present invention;

[0025] Figure 6 This is a schematic diagram of the first support rod and the second support rod of the present invention;

[0026] Figure 7 This is a schematic diagram of the connection scheme between the first blade plate, the second blade plate, and the second connecting ring body of the present invention.

[0027] Figure 8 This is a schematic diagram of the internal structure of the flow control component of the present invention;

[0028] Figure 9 This is a schematic diagram of the working process of an interference removal device for the determination of anions in high-salt seawater by ion chromatography.

[0029] Figure 10 This is a schematic diagram of the resin regeneration process of the present invention.

[0030] Explanation of reference numerals in the attached figures: 10. Chromatograph; 20. First frame; 21. Second frame; 30. Vacuum pump; 40. Controller; 50. First tube; 51. Flow meter; 52. Second tube; 53. Third tube; 60. Working column assembly; 61. Main pretreatment column; 62. Electromagnetic switching valve; 63. Secondary pretreatment column; 64. Collection container; 65. Feed chamber; 70. Spare column; 80. Auxiliary assembly; 81. First filter plate; 82. First support rod; 83. Second support rod; 84. First impeller; 85. First connecting ring; 86. Second connecting ring; 87. Second impeller; 88. Third connecting ring; 90. Flow control assembly; 91. First base; 92. Inlet chamber; 93. Sealing ring; 94. Rubber threaded sleeve; 95. Sliding plug; 96. First spring; 97. Guide plate. Detailed Implementation

[0031] The technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.

[0032] The concepts involved in this application will first be described with reference to the accompanying drawings. It should be noted that the following descriptions of various concepts are only for the purpose of making the content of this application easier to understand and do not constitute a limitation on the scope of protection of this application; furthermore, the embodiments and features in the embodiments of this application can be combined with each other unless otherwise specified. This application will now be described in detail with reference to the accompanying drawings and embodiments.

[0033] Example 1:

[0034] As shown in the attached figure Figure 9 Appendix Figure 1 - Appendix Figure 4 As shown, an interference removal device for the determination of anions in high-salt seawater by ion chromatography includes a working column group 60. The working column group 60 is connected to a chromatograph 10 through a delivery pipe. There are at least two working column groups 60. The upper end of each working column group 60 is connected to a first tube body 50, and an electrically controlled valve is provided at the connection. The working column group 60 includes a main pretreatment column 61 and a secondary pretreatment column 63 that are connected vertically.

[0035] This invention reduces the concentration of interfering elements in seawater by combining the main pretreatment column 61 and the secondary pretreatment column 63 in series, thus meeting the requirements for the detection of trace anions in ion chromatography and solving the problem of high-salt matrix masking the chromatographic signal. Furthermore, this invention uses a dual working column group 60 that can be dynamically switched according to usage requirements. That is, when one working column group 60 is performing ion removal, the other working column group 60 simultaneously completes backwashing, regeneration, and activation, avoiding the need to shut down the traditional single-column system.

[0036] Both the main pretreatment column 61 and the auxiliary pretreatment column 63 are filled with resin, but the cationic or anionic raw materials loaded in the main pretreatment column 61 and the auxiliary pretreatment column 63 are different. The different raw materials loaded in different resins enable the separate treatment of Cl... - and SO4 2⁻ Elements and cations work together to prevent overloading of a single resin column.

[0037] As shown in the attached figure Figure 3 As shown, there are at least two secondary pretreatment columns 63, and the main pretreatment column 61 is filled with functionalized Ag with a particle size of 40 μm. + The sulfonic acid-supported ion exchange resin, with at least one secondary pretreatment column 63 containing functionalized Ba with a particle size of 40 μm, is used. 2+ A cation-supported resin column, with at least one secondary pretreatment column 63 containing functionalized Na particles with a particle size of 40 μm. + A cation exchange resin-loaded column is used. At least two secondary pretreatment columns 63 are provided, forming a series flow with the main pretreatment column 61 to achieve Cl... - and SO4 2⁻ It also features stepwise removal of cations, avoiding the efficiency drop caused by loading too many types of ions onto a single resin column; at the same time, the modular resin column design allows for independent replacement of failed resins, reducing maintenance costs, and the column sequence can be flexibly adjusted according to seawater salinity fluctuations to adapt to different detection scenarios.

[0038] As shown in the attached figure Figure 4 As shown, a third tube 53 is connected to one side of both the main pretreatment column 61 and the secondary pretreatment column 63. The third tube 53 is connected to the side of both the main pretreatment column 61 and the secondary pretreatment column 63. When the pressure sensor or conductivity sensor detects a decrease in the performance of the resin column, the high-pressure chromatography pump can push backwash solution directionally to a single column through the third tube 53 to accurately dissolve the AgCl precipitate in the main pretreatment column 61 or the BaSO4 precipitate in the secondary pretreatment column 63, thus avoiding interference of the regeneration solution with other columns and improving regeneration efficiency.

[0039] As shown in the attached figure Figure 4 - Appendix Figure 7As shown, an auxiliary component 80 is built into the end of the main pretreatment column 61 near the third tube 53. The auxiliary component 80 includes two spaced-apart first filter plates 81. A first support rod 82 is fixedly connected to the bottom surface of the first filter plate 81, and a second support rod 83 is spaced apart on the side of the first support rod 82 and perpendicular to its axis. The two spaced-apart first filter plates 81 form a filter jacket, which can intercept particulate impurities in seawater, such as silt and biological debris, improve the rejection rate of solid particles ≥40μm, and prevent impurities from clogging the resin pores. At the same time, the porous structure of the filter plate allows the sample flow to be evenly dispersed to the resin layer, reducing local processing blind spots caused by fluid short circuits. Furthermore, the first support rod 82 is vertically fixed to the bottom surface of the filter plate, and the second support rod 83 is radially spaced and perpendicular to the first support rod 82, forming a support frame, which improves the load-bearing capacity of the filter plate, can withstand the fluid impact when pushed by the high-pressure chromatography pump, and prevents the filter plate from deforming and causing resin leakage.

[0040] Between two first filter plates 81, there are first leaf plates 84 arranged in a ring and second leaf plates 87 arranged in a ring. The first leaf plate 84 is connected to the surface of one of the first filter plates 81, and the second leaf plate 87 is connected to the surface of the other first filter plate 81. The first leaf plate 84 and the second leaf plate 87 are connected by a second connecting ring 86. There are at least three first leaf plates 84, which are arranged at intervals around the axis of the first filter plate 81. Adjacent first leaf plates 84 are fixed by a first connecting ring 85. There are at least three second leaf plates 87, which are arranged at intervals around the axis of the first filter plate 81. Adjacent second leaf plates 87 are fixed by a third connecting ring 88. The first connecting ring 85, the second connecting ring 86, and the third connecting ring 88 all have through holes in the middle.

[0041] At least three first blades 84 are arranged in a ring on one side of the first filter plate 81 and connected to at least three second blades 87 via second connecting rings 86, forming a multi-layered radial flow channel. When the sample flows through, it is cut into multiple fine streams by the blades, increasing the contact area between the fluid and the resin. Adjacent first blades 84 are fixed by first connecting rings 85, and adjacent second blades 87 are fixed by third connecting rings 88, forming a stable flow channel framework. This improves the uniformity of fluid distribution along the column radially, avoiding the situation where the flow velocity is high in the center and slow at the edge of the traditional column, ensuring a balanced resin utilization rate throughout the column. Furthermore, the through holes in the middle of the first connecting rings 85, second connecting rings 86, and third connecting rings 88 allow the fluid to pass axially, increasing the overall pressure drop compared to a bladeless structure. This maintains a stable flow rate even when pushed by a high-pressure chromatography pump, avoiding the risk of system overload due to excessive pressure drop.

[0042] The discharge end of the working column assembly 60 is equipped with a collection container 64. One end of the collection container 64 is connected to the sub-pretreatment column 63, and the other end is connected to the injection end of the chromatograph 10 through a delivery tube. The direct connection between one end of the collection container 64 and the discharge end of the sub-pretreatment column 63, and the connection between the other end and the injection end of the chromatograph 10 through a delivery tube, avoids the risk of contamination caused by traditional manual sample transfer and shortens the detection process time.

[0043] The first tube 50 is connected to a high-pressure chromatography pump, which delivers seawater samples to the working column assembly 60 through the first tube 50. The pump provides stable pressure, which pushes high-salt, high-viscosity seawater through the resin column quickly, thus shortening the pretreatment time for a single sample.

[0044] The working column assembly 60 is mounted on the second frame 21, which has a spare column 70 connected to the first tube 50. The bottom of the second frame 21 is connected to the first frame 20, on which the chromatograph 10 is mounted. The second frame 21 and the first frame 20 form a stable base through the bottom connection, preventing the tubing from loosening or the resin column from shifting due to vibration, and ensuring the stability of fluid transmission.

[0045] Both the main pretreatment column 61 and the auxiliary pretreatment column 63 are equipped with pressure sensors and conductivity sensors. After prolonged use of the resin column, the feedback from the pressure and conductivity sensor readings determines the performance degradation of the resin column, triggering and starting the regeneration system. A high-pressure chromatography pump pushes backwash solution to dissolve the precipitate in the resin column, followed by pure water rinsing, and then regeneration solution to activate and regenerate the resin column.

[0046] Example 2:

[0047] This embodiment provides an optimized solution based on Embodiment 1. See Appendix. Figure 1 As shown, the second frame 21 is vertically arranged and has two parallel uprights. The two uprights are mounted on the first frame 20 and connected by spaced horizontal bars. This allows for the installation of necessary components on the horizontal bars. The horizontal bars have clamps for assembling the working column assembly 60, fixing the working column assembly 60 to the uprights. In this embodiment, the working column assembly 60 can also be assembled and fixed to the horizontal bars by setting mounting plates or other methods. The two parallel uprights are vertically mounted on the first frame 20 and connected by horizontal bars to form a multi-layered installation plane. The unit floor space is reduced compared to a planar layout, and multiple components such as the working column assembly 60, spare column 70, and high-pressure chromatography pump can be integrated in a limited space. The working column assembly 60 is fixed to the horizontal bars by clamps or mounting plates. The disassembly and assembly time of a single column is shortened to less than 5 minutes, facilitating the rapid replacement of failed resin columns or adjustment of column sequence.

[0048] A controller 40 is fixed to the horizontal rod via an angle plate. The controller 40 is a PLC controller, which is connected to the electrically controlled valve, battery switching valve, flow meter 51, vacuum pump 30, sensors, and chromatograph 10 for precise control and program optimization. In this embodiment, the sensors are pressure sensors and conductivity sensors, but are not limited to these two types; they can also be temperature sensors, pH sensors, etc. The PLC controller 40 is connected to the electrically controlled valve and the solenoid switching valve 62, and can automatically switch between the working column group 60 and the standby column 70 according to a preset program. The column group switching response time is less than 1 second, avoiding sample processing interruptions caused by manual operation delays. Simultaneously, it activates the high-pressure chromatography pump to push the sample or regeneration solution at the set flow rate and pressure.

[0049] The device of the present invention supports multiple preset processing programs, such as high-salinity / low-salinity seawater modes, which can be switched with one click via a touch screen. The program switching time is less than 5 seconds, adapting to different detection needs. At the same time, it records operating data such as pressure, conductivity, and flow rate.

[0050] The first frame 20 has feet between its bottom and the ground. Preferably, shock-absorbing pads should be installed on the feet. Specifically, the feet are made of metal and are firmly connected to the bottom of the first frame 20. Each foot has a load-bearing capacity of ≥20kg to ensure that the device remains stationary when the high-pressure chromatography pump is working, and to avoid loosening of pipeline interfaces or displacement of the resin column due to shaking.

[0051] A vacuum pump 30 is installed on the second frame 21. The vacuum pump 30 is connected to the working column assembly 60 and the spare column 70 through the second tube 52. The vacuum pump 30 generates a controllable negative pressure through the second tube 52, which can assist the high-pressure chromatography pump in pushing low-viscosity seawater samples uniformly through the resin column, thereby reducing flow rate fluctuation errors. It is especially suitable for water samples with low salinity or low viscosity, avoiding the problem of uneven flow rate within the column caused by fluid gravity flow, and improving the stability of ion removal efficiency.

[0052] Example 3:

[0053] This embodiment provides an optimized solution based on Embodiment 1. See Appendix. Figure 3 As shown, the main pretreatment column 61 and the sub-pretreatment column 63 are connected by an electromagnetic switching valve 62. A third tube 53 is connected to one side of each of the main pretreatment column 61 and the sub-pretreatment column 63. The third tube 53 is connected to a backwash pump. In this embodiment, the backwash pump is a high-pressure chromatography pump. Figure 9 Appendix Figure 10As shown, pressure sensors and conductivity sensors in the main pretreatment column 61 and the auxiliary pretreatment column 63 perform real-time monitoring. When the pressure or conductivity exceeds the threshold, the controller 40 controls the backwash pump to work and simultaneously cuts off the working column group. Specifically, the working column group 60 is switched by means of an electronically controlled valve. The purpose is to keep one working column group 60 in working state while the other group performs backwash activation and regeneration to avoid downtime.

[0054] Example 4:

[0055] This embodiment provides an optimized solution based on Embodiment 1. See Appendix. Figure 4 As shown, the main pretreatment column 61 has a feed chamber 65 separated by a partition at its upper part, and the feed chamber 65 is connected to the first tube 50. The feed chamber 65 is separated from the resin layer of the main pretreatment column 61 by the partition. After the sample enters the chamber through the first tube 50, it is uniformly guided into the resin column by the flow control component 90 on the partition, which reduces the fluid impact velocity and avoids the resin particles from being displaced or broken due to the high-pressure sample flow directly scouring the resin surface.

[0056] A flow control component 90 is provided in the middle of the partition. The flow control component 90 includes a first base 91, which is a rotating structure with threads on its exterior and a rubber threaded sleeve 94. A threaded hole that mates with the rubber threaded sleeve 94 is provided on the partition. An inlet cavity 92 is provided in the middle of the surface of the first base 91. A limiting groove is provided at the bottom of the inlet cavity 92. A sealing ring 93 is filled in the limiting groove. A through hole penetrating the bottom of the first base 91 is provided below the limiting groove. A sliding plug 95 is filled in the through hole. An opening is provided in the middle of the sealing ring 93 to allow the end portion of the sliding plug 95 to pass through. The sliding plug 95 has an outer protruding ring in the middle. A guide plate 97 connected to its inner wall is fixedly connected in the through hole. Filter holes are provided on the surface of the guide plate 97. A first spring 96 is provided between the guide plate 97 and the outer protruding ring of the sliding plug 95. Inclined blades are arranged around the inner wall of the through hole.

[0057] The first substrate 91 of the present invention is installed on the partition plate by external thread and rubber threaded sleeve 94, which can prevent high pressure sample leakage. The sliding plug 95 is subjected to the dual action of sample pressure and the elastic force of the first spring 96 in the inlet cavity 92, which can automatically adjust the flow area of ​​the through hole and control the flow rate fluctuation within ±0.05mL / min. When the sample pressure increases or decreases, the flow area of ​​the through hole is controlled by the deformation of the first spring 96, so as to achieve adaptive adjustment of the flow rate from 0.1 to 5mL / min and avoid resin impact damage caused by sudden flow rate changes.

[0058] Furthermore, the filter holes on the surface of the guide plate 97 of the present invention can trap particulate impurities ≥50μm in the sample. At the same time, the gap between it and the outer protruding ring of the sliding plug 95 forms a turbulent region. Combined with the swirling effect generated by the inclined blades on the inner wall of the through hole, the uniformity of the sample flow velocity on the cross section of the resin column is improved, thereby improving the ion exchange efficiency.

[0059] It should also be noted that the terms "center," "upper," "lower," "left," "right," "vertical," "horizontal," "inner," and "outer," etc., indicate the orientation or positional relationship based on the orientation or positional relationship shown in the accompanying drawings, and are only for the convenience of describing this application and simplifying the description, and do not indicate or imply that the device or element referred to must have a specific orientation, or be constructed and operated in a specific orientation, and therefore should not be construed as a limitation on this application. Unless otherwise expressly specified and limited, the terms "installed," "connected," "linked," etc., should be interpreted broadly. For example, they can refer to a fixed connection, a detachable connection, or an integral connection; they can refer to a mechanical connection or an electrical connection; they can refer to a direct connection or an indirect connection through an intermediate medium; they can refer to the internal communication between two elements. For those skilled in the art, the specific meaning of the above terms in this application can be understood according to the specific circumstances.

[0060] The embodiments and / or implementation methods described above are merely preferred embodiments and / or implementation methods for implementing the technology of the present invention, and are not intended to limit the implementation methods of the technology of the present invention in any way. Any person skilled in the art can make some modifications or alterations to other equivalent embodiments without departing from the scope of the technical means disclosed in the content of the present invention, but they should still be regarded as the technology or embodiments that are substantially the same as the present invention.

[0061] This document uses specific examples to illustrate the principles and implementation methods of this application. The descriptions of the above embodiments are only for the purpose of helping to understand the methods and core ideas of this application. The above descriptions are only preferred embodiments of this application. It should be noted that due to the limitations of written expression, while there are objectively infinite specific structures, those skilled in the art can make several improvements, modifications, or changes without departing from the principles of this application, and can also combine the above technical features in an appropriate manner. These improvements, modifications, changes, or combinations, or the direct application of the inventive concept and technical solution to other situations without modification, should all be considered within the scope of protection of this application.

Claims

1. An interference removal device for the determination of anions in high-salinity seawater by ion chromatography, comprising a working column assembly (60), wherein the working column assembly (60) is connected to a chromatograph (10) via a delivery pipe, characterized in that, The working column group (60) is at least two, and the upper end of each working column group (60) is connected to the first pipe body (50), and an electric control valve is provided at the connection. The working column group (60) includes a main pretreatment column (61) and a secondary pretreatment column (63) that are connected vertically. The main pretreatment column (61) and the secondary pretreatment column (63) are respectively connected to a third tube (53) on one side. The main pretreatment column (61) has an auxiliary component (80) built into one end near the third tube (53). The auxiliary component (80) includes two spaced first filter plates (81). The bottom surface of the first filter plate (81) is fixedly connected to a first support rod (82). The first support rod (82) is provided with a second support rod (83) spaced apart on the side and perpendicular to its axis. Between the two first filter plates (81), there is a first leaf plate (84) arranged in a ring and a second leaf plate (87) arranged in a ring. The first leaf plate (84) is connected to the surface of one of the first filter plates (81), and the second leaf plate (87) is connected to the surface of the other first filter plate (81). The first leaf plate (84) and the second leaf plate (87) are connected by a second connecting ring (86).

2. The interference removal device for the determination of anions in high-salinity seawater by ion chromatography according to claim 1, characterized in that, Both the main pretreatment column (61) and the secondary pretreatment column (63) are filled with resin, and the cationic or anionic raw materials loaded in the main pretreatment column (61) and the secondary pretreatment column (63) are different.

3. The interference removal device for the determination of anions in high-salinity seawater by ion chromatography according to claim 1, characterized in that, There are at least two sub-pretreatment columns (63), and each of the main pretreatment columns (61) is filled with functionalized Ag+-loaded sulfonic acid ion exchange resin. At least one of the sub-pretreatment columns (63) has a functionalized Ba2+-loaded cation resin column, and at least one of the sub-pretreatment columns (63) has a functionalized Na+-loaded cation resin column.

4. The interference removal device for the determination of anions in high-salinity seawater by ion chromatography according to claim 1, characterized in that, The discharge end of the working column group (60) is provided with a collection container (64). One end of the collection container (64) is connected to the sub-pretreatment column (63), and the other end is connected to the injection end of the chromatograph (10) through a delivery tube.

5. The interference removal device for the determination of anions in high-salinity seawater by ion chromatography according to claim 1, characterized in that, The first tube (50) is connected to a high-pressure chromatography pump.

6. The interference removal device for the determination of anions in high-salinity seawater by ion chromatography according to claim 1, characterized in that, The working column assembly (60) is installed on the second frame (21), and the second frame (21) is provided with a spare column (70) that communicates with the first tube (50). The bottom of the second frame (21) is connected to the first frame (20), and the chromatograph (10) is installed on the first frame (20).

7. The interference removal device for the determination of anions in high-salinity seawater by ion chromatography according to claim 1, characterized in that, Pressure sensors and conductivity sensors are installed in both the main pretreatment column (61) and the secondary pretreatment column (63).

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