Impurity acquisition system, quality inspection system, and liquid production and supply system

Abstract

An impurity acquisition system is provided with: a concentration column (200) that adsorbs impurities in a liquid to be inspected; and a control device (700) that switches between a concentration step in which a liquid to be inspected is introduced to the concentration column (200), an eluent filling step in which a filling container (503) is filled with a given amount of an eluent (502) that elutes impurities adsorbed to the concentration column (200), and an elution recovery step in which the eluent (502) is filled with a given amount of the eluent (502) that recovers impurities adsorbed to the concentration column (200). The eluent filled in the filling container (503) is introduced to a concentration column (200) and recovered to a recovery container.

Description

Technical Field

[0001] The invention relates to an impurity acquisition system, a quality inspection system and a liquid manufacturing supply system. Background Art

[0002] Generally, as one of the methods for inspecting the quality of ultrapure water supplied from an ultrapure water production facility to a point of use (e.g., a point of use in a semiconductor cleaning device), there is an analysis method using a concentration method using an ion exchanger. As an analysis method based on such a concentration method, there is a method that allows ultrapure water to flow through an ion exchanger for a given period of time, removes and recovers the ion exchanger, and elutes impurities from the recovered ion exchanger to measure their concentration, thereby inspecting the quality of the ultrapure water (e.g., see Patent Document 1).

[0003] Prior art literature

[0004] Patent Literature

[0005] Patent Document 1: Japanese Patent Application Publication No. 2001-153854 Summary of the invention

[0006] Technical problem to be solved by the invention

[0007] In the above-mentioned techniques, the ion exchanger must be removed in order to inspect the quality of ultrapure water, which is laborious and does not allow efficient inspection.

[0008] An object of the present invention is to provide an impurity acquisition system, a quality inspection system, and a liquid production and supply system capable of efficiently inspecting the quality of a liquid.

[0009] Technical solutions for solving technical problems

[0010] The impurity acquisition system of the present invention is an impurity acquisition system for acquiring impurities in a liquid to be inspected, and has:

[0011] A first adsorber that adsorbs impurities in the liquid to be inspected; and

[0012] A first control device switches between a concentration process, an eluent filling process and an elution recovery process. In the concentration process, the liquid to be inspected is passed to the first adsorbent. In the eluent filling process, a given amount of eluent is filled into a filling container, and the eluent elutes impurities adsorbed on the first adsorbent. In the elution recovery process, the eluent filled in the filling container is passed to the first adsorbent and recovered to a recovery container.

[0013] In addition, the quality inspection system of the present invention comprises:

[0014] A first adsorber that adsorbs impurities in the liquid to be inspected; an impurity acquisition system having a first control device, the first control device switching a concentration process, an eluent filling process, and an elution recovery process, wherein in the concentration process, the liquid to be inspected is passed to the first adsorber, in the eluent filling process, a given amount of eluent is filled into a filling container, and the eluent elutes impurities adsorbed on the first adsorber, and in the elution recovery process, the eluent filled in the filling container is passed to the first adsorber and recovered into a recovery container;

[0015] an information processing device for detecting the amount of impurities in the eluate after passing through the first adsorber; and

[0016] The processing device calculates the amount of impurities in the liquid to be inspected.

[0017] In addition, the liquid production and supply system of the present invention comprises:

[0018] A first adsorber that adsorbs impurities in the liquid to be inspected; an impurity acquisition system having a first control device, the first control device switching a concentration process, an eluent filling process, and an elution recovery process, wherein in the concentration process, the liquid to be inspected is passed to the first adsorber, in the eluent filling process, a given amount of eluent is filled into a filling container, and the eluent elutes impurities adsorbed on the first adsorber, and in the elution recovery process, the eluent filled in the filling container is passed to the first adsorber and recovered into a recovery container;

[0019] an information processing device for detecting the amount of impurities in the eluate after passing through the first adsorber; and

[0020] A calculation processing device, which calculates the amount of impurities in the liquid to be inspected;

[0021] a valve portion that controls supply of the liquid to be inspected from a liquid manufacturing and supplying device that performs at least one of manufacturing and supplying the liquid to be inspected to a use point that uses the liquid to be inspected; and

[0022] A second control device controls the valve portion based on the amount of foreign matter in the liquid to be inspected calculated by the arithmetic processing device.

[0023] Effects of the Invention

[0024] According to the present invention, it is possible to efficiently inspect the quality of liquid. BRIEF DESCRIPTION OF THE DRAWINGS

[0025] Figure 1 It is a diagram showing a first embodiment of the impurity acquisition system of the present invention.

[0026] Figure 2 It is used to illustrate Figure 1 A flowchart of an example of an impurity acquisition method in the impurity acquisition system shown.

[0027] Figure 3 It is used to illustrate Figure 2 This is a flowchart of an example of the processing of the concentration step in step S1 in the flowchart shown.

[0028] Figure 4 It is used to illustrate Figure 2 This is a flowchart of an example of the processing of the purge step in step S2 in the flowchart shown.

[0029] Figure 5 It is used to illustrate Figure 2 This is a flowchart of an example of the processing of the eluent filling step of step S3 in the flowchart shown.

[0030] Figure 6 It is used to illustrate Figure 2 This is a flowchart of an example of the processing of the elution recovery step of step S4 in the flowchart shown.

[0031] Figure 7 It is used to illustrate Figure 2 This is a flowchart of an example of the processing of the cleaning step of step S5 in the flowchart shown.

[0032] Figure 8 It is a diagram showing a second embodiment of the impurity acquisition system of the present invention.

[0033] Fig. 9 It is used to illustrate Figure 8 A flowchart of an example of an impurity acquisition method in the impurity acquisition system shown.

[0034] Fig.10 It is used to illustrate Fig. 9 This is a flowchart of an example of the processing of the regeneration liquid filling step of step S26 in the flowchart shown.

[0035] Fig.11 It is used to illustrate Fig. 9 This is a flowchart of an example of processing of the regeneration step in step S27 in the flowchart shown.

[0036] Fig.12 It is a diagram showing a third embodiment of the impurity acquisition system of the present invention.

[0037] Fig.13 It is used to illustrate Fig.12 A timing chart showing an example of timing control between systems performed by the control device shown.

[0038] Fig.14 This is a diagram showing an example of a liquid production and supply system to which the impurity acquisition system of the present invention is applied.

[0039] Fig.15 It is used to illustrate Fig.14 A flowchart of an example of processing in the system shown.

[0040] Fig.16 This is a diagram showing another example of a liquid production and supply system to which the impurity acquisition system of the present invention is applied. DETAILED DESCRIPTION

[0041] Hereinafter, embodiments of the present invention will be described with reference to the accompanying drawings. Here, the description will be given by taking the case where the liquid to be inspected is ultrapure water as an example.

[0042] (First Embodiment)

[0043] Figure 1 FIG. 1 is a diagram showing a first embodiment of the impurity acquisition system of the present invention. Figure 1 As shown, the impurity acquisition system in this embodiment has a concentration column (ion exchanger unit) 200 as a first adsorbent, a protection column 210 as a second adsorbent, valves 301 to 306 as valves, a cumulative flow meter 411, a container 501 storing an eluent 502, a filling container 503, a recovery container 504 and a control device 700.

[0044] The concentrating column 200 is a unit that adsorbs impurities from a liquid to be inspected from an ultrapure water manufacturing device. Here, the ultrapure water manufacturing device, for example, manufactures ultrapure water to be supplied to a semiconductor cleaning device as a point of use, and supplies the ultrapure water to the semiconductor cleaning device. In the following description, the ultrapure water is indicated as a liquid to be inspected (liquid to be inspected), and the liquid to be inspected is ultrapure water supplied from the ultrapure water manufacturing device. The concentrating column 200 can be made of any material that has an ion removal or ion adsorption function. As examples of the concentrating column 200, an ion adsorption membrane, an integral organic porous body, or an ion exchange resin can be cited. The object to be removed or adsorbed by the concentrating column 200 is an impurity. The impurities include ions (ionic metal impurities) and substances in the form of particles. In this embodiment, the functional group of the concentrating column 200 is a cation exchange group, an anion exchange group, or a chelating compound.

[0045] As a concentration method using the concentration column 200 of the present invention, for example, a concentration method using a monolithic organic porous body is adopted. Examples of the structure of the monolithic organic porous body used here include the continuous bubble structure disclosed in Japanese Patent Publication No. 2002-306976 and Japanese Patent Publication No. 2009-62512, the co-continuous structure disclosed in Japanese Patent Publication No. 2009-67982, the particle agglomeration structure disclosed in Japanese Patent Publication No. 2009-7550, and the particle composite structure disclosed in Japanese Patent Publication No. 2009-108294. In addition, as the structure, material, and properties of the ion exchanger, the ion exchanger disclosed in Japanese Patent Publication No. 2019-195763 can be cited. In addition, in the monolithic organic porous body, the ion exchange groups introduced into the monolithic organic porous body cation exchanger, and the anion exchange groups introduced into the monolithic organic porous body anion exchanger include the groups disclosed in Japanese Patent Application Publication No. 2019-195763.

[0046] The protective column 210 is a material that absorbs impurities from the liquid to be inspected from the ultrapure water production equipment. The protective column 210 can be any material as long as it can absorb and remove impurities from the liquid to be inspected, and can be the same as the concentrating column 200, for example.

[0047] Valve 301 is an on-off valve that controls the passage of the liquid to be inspected and the liquid used in cleaning from the ultrapure water manufacturing equipment to the impurity acquisition system. Valve 301 is an acquisition unit that is used to obtain the liquid to be inspected from the path from the ultrapure water manufacturing equipment to the semiconductor cleaning device. Valve 302 is a valve that is controlled in the following manner: any one of the paths passing through the guard column 210 and the path not passing through the guard column 210 is controlled, and the path is used as a path for the liquid (liquid to be inspected, liquid used in cleaning) from valve 301 to valve 303. Valve 303 is a valve that is controlled in the following manner: the liquid from valve 302 is controlled to pass to any one of valve 304 and the drainage path, and valve 303 controls the liquid from valve 304 to pass to the drainage path. Valve 304 is a valve that is controlled in the following manner: the liquid from valve 303 is controlled to pass to the concentration column 200, or the eluent from the concentration column 200 is controlled to pass to the recovery container 504. The valve 305 is a valve controlled so that any of the liquid (eluent) passed from the filling container 503 or the gas from the valve 306 is passed to the concentrating column 200, or the liquid from the concentrating column 200 is passed to the valve 306. The valve 306 is a valve controlled so that the liquid passed from the valve 305 is passed to the drainage path provided with the integrating flow meter 411, or the gas (for example, nitrogen) supplied in the purge process or the liquid displaced by the gas is discharged to the valve 305. These valves are opened and closed and the path is selected according to the control signal from the control device 700. In addition, as the valves 302 to 306, for example, a three-way valve can be used.

[0048] The eluent 502 is an acidic or alkaline aqueous solution, and elutes the impurities concentrated in the concentration column 200. Examples of the eluent 502 include acidic aqueous solutions such as nitric acid, hydrochloric acid, and sulfuric acid, and alkaline aqueous solutions of organic bases such as tetramethylammonium hydroxide (TMAH). The eluent 502 is an aqueous solution having a metal impurity concentration of less than 100 ng / L. The dilution degree of the eluent 502 is not particularly limited. The eluent 502 may also be an aqueous solution diluted with the test object water of the measurement object.

[0049] The recovery container 504 is a container into which the eluent flows via the valve 304 in the elution recovery process, and the eluent contains impurities eluted from the concentrating column 200. As the recovery container 504, for example, a recovery bottle can be cited. The recovery container 504 is not particularly limited as long as it can recover the eluent. The filling container 503 is a container used in the elution recovery process. A given amount of eluent is filled in the filling container 503. The filling container only needs to have a structure that can be filled with liquid. As the filling container 503, for example, a tube, a bottle, a tank, etc. can be cited. In the case where the filling container 503 is a tube, the shape of the filling container 503 can also be annular. As the filling container 503, a container made of a resin material with little dissolution of metal impurities can be cited. The filling container 503 is preferably composed of fluorine-based materials such as PFA, PTFE, and PVDF. By setting the filling container 503 as a tube, it can be directly connected to the components of the front and rear stages arranged in the filling container 503, and the number of parts can be reduced. The filling method of the given amount of eluent to the filling container 503 may be a gas pressure feeding method or a method of conveying the eluent 502 from the container 501 using a pump. In addition, as to whether the filling amount of the eluent to the filling container 503 is the given amount, for example, a measuring device for measuring the filling amount of the eluent to the filling container 503, a sensor for detecting the filling of the given amount, or a weight meter for measuring the weight of the given amount of eluent may be used for determination. The cumulative flow meter 411 measures the flow rate of the liquid flowing out as drainage. The value measured by the cumulative flow meter 411 is notified to the control device 700. This notification may also use a given signal. Alternatively, the cumulative flow meter 411 may send the signal and the control device 700 may receive the signal.

[0050] The control device 700 is a first control device, which controls the opening and closing of each valve 301 to valve 306 and the start / end of filling the eluent 502 into the filling container 503 based on a preset time. The passage of the given period can also be determined based on whether the preset time has passed. In addition, the control device 700 can also control the opening and closing of each valve 301 to valve 306 based on whether the amount of liquid (liquid to be inspected) measured by the cumulative flow meter 411 reaches a preset value (threshold value). In addition, the control device 700 can also control the start and end of filling the eluent 502 into the filling container 503 by controlling the gas pressure delivery and pump based on the detection results of the above-mentioned sensors, the measurement results of the weight meter, etc.

[0051] The following, Figure 1 The impurity acquisition method in the impurity acquisition system shown in FIG. Figure 2 It is used to illustrate Figure 1 A flowchart of an example of an impurity acquisition method in the impurity acquisition system shown.

[0052] First, the control device 700 performs a concentration process (step S1 ). Figure 3 It is used to illustrate Figure 2 Flowchart of an example of the processing of the concentration process of step S1 in the flowchart shown. The control device 700 controls the valve 302 so that the liquid to be inspected from the valve 301 goes to the path leading to the valve 303 without passing through the protection column 210 (step S111). The control device 700 controls the valve 303 so that the liquid to be inspected from the valve 302 goes to the path leading to the valve 304 (step S112). The control device 700 controls the valve 304 so that the liquid to be inspected from the valve 303 passes to the concentration column 200 (step S113). The control device 700 controls the valve 305 so that the liquid to be inspected passed into the concentration column 200 goes to the path leading to the valve 306 (step S114). The control device 700 controls the valve 306 so that the liquid to be inspected from the valve 305 goes to the drainage path via the integrating flow meter 411 (step S115). If the control of steps S111 to S115 is completed, a path is established through valve 301, valve 302, valve 303, valve 304, concentrating column 200, valve 305, valve 306 and cumulative flow meter 411. Here, the control device 700 temporarily controls the opening and closing state of valve 301 to a closed state so that the liquid to be inspected from the ultrapure water manufacturing equipment does not flow into this system. Next, the control device 700 resets the cumulative flow meter 411 (step S116). Then, the control device 700 controls the opening and closing state of valve 301 to an open state so that the liquid to be inspected from the ultrapure water manufacturing equipment flows into this system. Thereafter, the control device 700 determines whether the value of the flow measured by the cumulative flow meter 411 reaches a given threshold value (step S117). If the value of the flow measured by the cumulative flow meter 411 reaches a given threshold value, the control device 700 performs the process of step S2.

[0053] The control device 700 executes a purge process (step S2). In the purge process, gas is injected into the pipe (path) and the like to treat the pipe, so that impurities, water, and the like remaining in the pipe and the like flow out. Figure 4 It is used to illustrate Figure 2Flowchart of an example of the processing of the purge process of step S2 in the flowchart shown. The control device 700 controls the valve 306 so that the gas (e.g., nitrogen) supplied from the outside is supplied to the path leading to the valve 305 (step S121). As the types of gas used here, inert gas, air (atmosphere), oxygen, etc. can be listed. As inert gas, rare gases such as nitrogen, argon, and helium can be listed. The purity of the gas is preferably 99.9% or more, and more preferably 99.99% or more. The less impurities in the gas, the more preferred the purity. In the case where the gas is an inert gas, the impurities contained in the high-purity gas are methane, oxygen, carbon dioxide, moisture, etc., and in the case where the gas is air and oxygen, the impurities contained in the high-purity gas are particles, moisture, etc. The control device 700 controls the valve 303 so that the gas from the valve 304 and the liquid pushed out by the gas are discharged to the drainage path (step S122). If the control of steps S121 and S122 is completed, a path is established through valve 306, valve 305, concentrating column 200, valve 304, and valve 303. Next, gas is injected for purging. After that, the control device 700 determines whether the purging is completed (step S123). This determination can be based on the elapsed time, or it can be based on the amount of gas injected after the path is opened, wherein the elapsed time is the time elapsed after the valve 306, valve 305, valve 304, and valve 303 are temporarily closed at the start of the purge and then opened, and the path is opened. When the purge is completed, the control device 700 performs the process of step S3.

[0054] The control device 700 executes an eluent filling step (step S3 ). Figure 5 It is used to illustrate Figure 2 Flowchart of an example of the processing of the eluent filling process of step S3 in the flowchart shown. The control device 700 starts to fill the eluent 502 stored in the container 501 into the filling container 503 (step S131). For example, the control device 700 uses gas pressure feeding and a pump to transport the eluent 502 from the container 501 to the filling container 503. Then, the control device 700 determines whether the filling amount of the eluent 502 to the filling container 503 has reached a given amount (step S132). This determination can also be made based on the detection results of the above-mentioned sensors, the measurement results of the weight meter, etc. If it is determined that the filling amount of the eluent 502 to the filling container 503 has reached a given amount, the control device 700 ends the filling of the eluent (step S133) and performs the process of step S4.

[0055] The control device 700 executes the elution recovery step (step S4). Figure 6 It is used to illustrate Figure 2Flowchart of an example of the processing of the elution recovery step of step S4 in the flowchart shown in FIG. In this step, the impurities in the concentration column 200 are eluted using the predetermined amount of eluent filled in the filling container 503 in the eluent filling step of step S3. The control device 700 controls the valve 305 so that the eluent filled in the filling container 503 is passed to the concentration column 200 (step S141). At this time, the control device 700 controls so that the eluent 502 stored in the container 501 is not supplied to the filling container 503. For example, an on-off valve may be provided between the container 501 and the filling container 503, and the control device 700 controls the on-off state of the on-off valve to be closed. The control device 700 controls the valve 304 so that the eluent passing through the concentration column 200 is recovered to the recovery container 504 (step S142). When the control of steps S141 and S142 is completed, a path from the filling container 503 to the recovery container 504 via the valve 305, the concentrating column 200, and the valve 304 is established. The control device 700, for example, uses gas pressure feeding or a pump to convey the eluent from the filling container 503 to the recovery container 504. When the recovery of the eluent in the recovery container 504 is completed (step S143), the control device 700 performs the process of step S5. As for determining whether the recovery of the eluent in the recovery container 504 is completed, for example, when the supply of the eluent from the filling container 503 is detected to be gone, the control device 700 determines that the recovery of the eluent in the recovery container 504 is completed. In this elution recovery process, the direction in which the eluent is passed to the concentrating column 200 is the opposite direction to the direction in which the liquid to be inspected is passed to the concentrating column 200 in the concentration process. The amount (including concentration) of impurities contained in the liquid to be inspected passed through the concentrating column 200 in the concentration process decreases with the direction of passing the liquid. Therefore, by passing the eluent in the direction opposite to the direction in which the liquid to be inspected is passed through the concentrating column 200 in the concentration process, a high recovery rate can be obtained using a smaller amount of eluent.

[0056] The control device 700 executes a cleaning process (step S5). Figure 7 It is used to illustrate Figure 2Flowchart of an example of the processing of the cleaning process of step S5 in the flowchart shown. The control device 700 controls the valve 302 so that the liquid to be inspected from the valve 301 goes to the protection column 210 (step S151). The control device 700 controls the valve 303 so that the liquid to be inspected from the protection column 210 goes to the path leading to the valve 304 (step S152). The control device 700 controls the valve 304 so that the liquid to be inspected from the valve 303 passes through the concentrating column 200 (step S153). The control device 700 controls the valve 305 so that the liquid to be inspected that has passed into the concentrating column 200 goes to the path leading to the valve 306 (step S154). The control device 700 controls the valve 306 so that the liquid to be inspected from the valve 305 is discharged to the drainage path via the integrating flow meter 411 (step S155). If the control of steps S151 to S155 is completed, a path is established through valve 301, valve 302, protective column 210, valve 303, valve 304, concentrating column 200, valve 305, valve 306 and cumulative flow meter 411. Here, the control device 700 temporarily controls the opening and closing state of valve 301 to a closed state so that the liquid to be inspected from the ultrapure water manufacturing equipment does not flow into this system. Next, the control device 700 resets the cumulative flow meter 411 (step S156). Then, the control device 700 controls the opening and closing state of valve 301 to an open state so that the liquid to be inspected from the ultrapure water manufacturing equipment flows into this system. Thereafter, the control device 700 determines whether the value of the flow measured by the cumulative flow meter 411 reaches a given threshold value (step S157). If the value of the flow measured by the cumulative flow meter 411 reaches a given threshold value, the control device 700 performs the process of step S1.

[0057] Thus, in this method, by controlling valves and pumps provided at important positions of the path every given period, the concentration process, which uses the concentration column 200 to capture impurities in the liquid to be inspected, the elution recovery process, which elutes and recovers the captured impurities from the concentration column 200, and the cleaning process, which cleans the concentration column 200 after the impurities have been eluted with the liquid to be inspected. Thus, a sample for inspecting the water quality of the inspection target water can be obtained without removing the concentration column 200 from the system. As a result, the water quality of the inspection target water can be inspected efficiently. In addition, when the elution recovery process is performed after the concentration column 200 is removed from the system, the concentration column 200 may be contaminated when the concentration column 200 is removed or when the concentration column 200 is installed in the device for elution, and the inspection accuracy may be reduced. In this method, the elution recovery process can be repeatedly performed without removing the concentration column 200 from the system. Therefore, the concentration column 200 is not contaminated, and the reduction of the inspection accuracy can be suppressed. Further, the eluent used in the eluent recovery process is used only in a predetermined amount and is recovered in a container for analysis. As a method for continuous analysis, there is a flow injection method (FIA method) in which the eluent is directly introduced into a detector (analyzer). In the FIA ​​method, the impurity concentration is calculated using the peak area derived from the retention time and the variation. In the FIA ​​method, the retention time of each impurity is different. Therefore, it is necessary to select an eluent for each impurity detected, and in addition, it is necessary to change the measurement mode of the detector according to the impurity. As a result, there is a technical problem that it is difficult to simultaneously detect multiple impurities from the eluent obtained in one process. On the other hand, in this method, a certain amount of eluent is used, and impurities are detected after being recovered to a container. Therefore, in this method, multiple impurities can be detected simultaneously from the eluent obtained in one process, and the technical problems of the above-mentioned FIA method can be solved. It should be noted that the control device 700 can also perform only one of the purge process and the eluent filling process. In addition, the control device 700 can also fill the eluent in a component other than the filling container 503 in the eluent filling process. In this case, the control device 700 recovers the eluent filled in the member in the eluent recovery process. It should be noted that the control device 700 may also perform a pipeline cleaning process before the concentration process, and the pipeline cleaning process cleans the path through the valve 301, the valve 302, the protective column 210 and the valve 303. By providing the pipeline cleaning process, the accumulated water in the piping between the ultrapure water manufacturing equipment and the impurity acquisition system can be discharged. Therefore, it is possible to transfer to the concentration process in the state where water is passed from the ultrapure water manufacturing equipment.

[0058] (Second Embodiment)

[0059] Figure 8 FIG. 2 is a diagram showing a second embodiment of the impurity acquisition system of the present invention. Figure 8 As shown, the impurity acquisition system in this method is Figure 1 In addition to the components in the embodiment shown in FIG. 3 , the valve 307, a container 505 storing a regeneration liquid 506, and a filling container 507 are also provided. Figure 8 As shown, the impurity acquisition system in this embodiment has a control device 701 to replace Figure 1 A control device 700 is shown in the manner shown.

[0060] The regeneration liquid 506 is an acidic or alkaline liquid, and is used to regenerate the concentration column 200 in the regeneration step after eluting and cleaning the impurities concentrated in the concentration column 200. The regeneration liquid 506 is placed in a container such as a bottle such as the container 505. The metal impurity concentration of the regeneration liquid 506 is less than 100 ng / L.

[0061] The filling container 507 is a container filled with a predetermined amount of regeneration liquid used in the regeneration process. The components of the filling container 507 may be the same as those of the filling container 503. The method of filling the predetermined amount of regeneration liquid to the filling container 507 may also be a method of sending the regeneration liquid 506 from the container 505 by gas pressure or by using a pump. In addition, as to whether the filling amount of the regeneration liquid to the filling container 507 is the predetermined amount, for example, a measuring device for measuring the filling amount of the regeneration liquid to the filling container 507, a sensor for detecting the filling of the predetermined amount, or a weight meter for measuring the weight of the predetermined amount of regeneration liquid can be used for determination.

[0062] The valve 307 is a valve controlled so that either the gas from the valve 306 or the liquid (regeneration liquid) introduced from the filling container 507 is passed to the concentrating column 200, or the liquid from the concentrating column 200 via the valve 305 is passed to the valve 306. The valve 307 is opened and closed and the path is selected according to a control signal from the control device 701. As the valve 307, for example, a three-way valve is used.

[0063] The control device 701 is a first control device, which controls the opening and closing of each of the valves 301 to 307 and the start / end of the filling of the eluent 502 and the regeneration liquid 506 into the filling container 503 and the filling container 507 based on a preset time. The control device 701 can also control the opening and closing of each of the valves 301 to 307 based on whether the amount of the liquid (liquid to be inspected) measured by the cumulative flow meter 411 reaches a preset value (threshold value). In addition, the control device 701 can also control the start and end of the filling of the eluent 502 and the regeneration liquid 506 by controlling the gas pressure delivery and the pump based on the detection results of the above-mentioned sensors, the measurement results of the weight meter, etc.

[0064] The following, Figure 8The impurity acquisition method in the impurity acquisition system shown in FIG. Fig. 9 It is used to illustrate Figure 8 A flowchart of an example of an impurity acquisition method in the impurity acquisition system shown.

[0065] First, the control device 701 performs a concentration process (step S21). This process is the same as the concentration process in the first embodiment. Then, the control device 701 performs a purge process (step S22). This process is the same as the purge process in the first embodiment. Then, the control device 701 performs an eluent filling process (step S23). This process is the same as the eluent filling process in the first embodiment. Then, the control device 701 performs an elution recovery process (step S24). This process is the same as the elution recovery process in the first embodiment. Then, the control device 701 performs a cleaning process (first cleaning process) (step S25). This process is the same as the cleaning process in the first embodiment.

[0066] Next, the control device 701 executes a regeneration liquid filling process (step S26). Fig.10 It is used to illustrate Fig. 9 Flowchart of an example of the processing of the regeneration liquid filling process of step S26 in the flowchart shown. The control device 701 starts to fill the regeneration liquid 506 stored in the container 505 into the filling container 507 (step S261). For example, the control device 701 uses gas pressure feeding and a pump to transport the regeneration liquid 506 from the container 505 to the filling container 507. Then, the control device 701 determines whether the filling amount of the regeneration liquid 506 to the filling container 507 has reached a given amount (step S262). This determination can also be made based on the detection results of the above-mentioned sensors, the measurement results of the weight meter, etc. If it is determined that the filling amount of the regeneration liquid 506 has reached a given amount, the control device 701 ends the filling of the regeneration liquid (step S263) and performs the process of step S27.

[0067] The control device 701 executes the regeneration process (step S27). Fig.11 It is used to illustrate Fig. 91 is a flowchart of an example of processing of the regeneration process of step S27 in the flowchart shown in FIG. 1. In this process, the concentrating column 200 is regenerated using a predetermined amount of regeneration liquid filled in the filling container 507 in the regeneration liquid filling process of step S26. The control device 701 controls the valve 307 so that the regeneration liquid filled in the filling container 507 passes through the valve 307 to the concentrating column 200 (step S271). At this time, the control device 701 controls so that the regeneration liquid 506 stored in the container 505 is not supplied to the filling container 507. For example, an on-off valve may be provided between the container 505 and the filling container 507, and the control device 701 controls the on-off state of the on-off valve to be closed. The control device 701 controls the valve 303 so that the regeneration liquid from the valve 304 is discharged to the drainage path (step S272). When the control of steps S271 and S272 is completed, a path is established for the regeneration liquid to flow and be discharged from the filling container 507 via the valve 307, the valve 305, the concentrating column 200, the valve 304, and the valve 303. The control device 701, for example, uses gas pressure feeding or a pump to transfer the regeneration liquid from the filling container 507 to the concentrating column 200. When the transfer of the regeneration liquid filled in the filling container 507 is completed (step S273), the control device 701 performs the process of step S28. As for determining whether the transfer of the regeneration liquid filled in the filling container 507 is completed, for example, when the supply of the regeneration liquid from the filling container 507 is detected to be stopped using a sensor or the like, the control device 701 determines that the transfer of the regeneration liquid filled in the filling container 507 is completed. The direction in which the regeneration liquid is passed to the concentrating column 200 in this regeneration process is the opposite direction to the direction in which the liquid to be inspected is passed to the concentrating column 200 in the concentrating process.

[0068] The control device 701 performs a cleaning process (second cleaning process) (step S28). This process is the same as the cleaning process of step S25. After the process of step S28 is completed, the control device 701 performs the process of step S21.

[0069] Thus, in this method, by controlling valves and pumps provided at important positions of the path every given period, the concentration process, which uses the concentration column 200 to capture impurities in the liquid to be inspected, the elution recovery process, which elutes and recovers the captured impurities from the concentration column 200, and the cleaning process, which cleans the concentration column 200 after the impurities have been eluted with the liquid to be inspected. Thus, a sample for inspecting the water quality of the inspection target water can be obtained without removing the concentration column 200 from the system. As a result, the water quality of the inspection target water can be inspected efficiently. In addition, when the elution recovery process is performed after the concentration column 200 is removed from the system, the concentration column 200 may be contaminated when the concentration column 200 is removed or when the concentration column 200 is installed in the device for elution, and the inspection accuracy may be reduced. In this method, the elution recovery process can be performed without removing the concentration column 200 from the system. Therefore, the concentration column 200 is not contaminated, and the reduction of the inspection accuracy can be suppressed. Furthermore, the eluent used in the eluent recovery process is used only in a predetermined amount. Thus, since the analysis is performed after a certain amount is recovered, the impurity concentration in the eluent becomes a uniform value that does not change over time, and an accurate value can be obtained. It should be noted that the control device 701 may also perform only one of the purging process and the eluent filling process. In addition, the control device 701 may also fill the eluent in a component other than the filling container 503 in the eluent filling process. In this case, the control device 701 recovers the eluent filled in the component in the eluent recovery process. In addition, the amount of regeneration liquid used by the control device 701 in the regeneration process is only a predetermined amount. Thus, the regeneration liquid can be used without waste in the regeneration process. In the step of temporarily removing the concentrating column 200 and regenerating and installing it, which is usually performed, when the concentrating column 200 is removed and when the concentrating column 200 is installed in the device for regeneration, the concentrating column 200 may be contaminated. As a result, the inspection accuracy may be reduced. In this embodiment, the regeneration process can be repeatedly performed without removing the concentrating column 200 from the system. Therefore, the time for removal and installation can be saved, the concentrating column 200 is not contaminated, and the reduction in inspection accuracy can be suppressed.

[0070] (Third Embodiment)

[0071] Fig.12 FIG. 2 is a diagram showing a third embodiment of the impurity acquisition system of the present invention. Fig.12As shown, the impurity acquisition system in this embodiment has concentration columns 200-1 to 200-3, valves 301-1 to 301-3, valves 304-1 to 304-3, valves 305-1 to 305-3, containers 501-1 to 501-3 storing eluents 502-1 to 502-3, respectively, filling containers 503-1 to 503-3, recovery containers 504-1 to 504-3, and a control device 702. That is, the impurity acquisition system in this embodiment is a method in which the components of the impurity acquisition system in the first embodiment are arranged in parallel as three systems. Fig.12 In the figure, for the convenience of illustration, other valves and flow meters in the first embodiment are omitted. Concentrating columns 200-1 to 200-3 are respectively equivalent to concentrating columns 200. Valves 301-1 to 301-3 are respectively equivalent to valve 301. Each valve 301-1 to 301-3 is set at different points where the liquid to be inspected is concentrated using the concentrating columns 200-1 to 200-3. These points are arbitrary positions on the path (pipeline direction) from the ultrapure water manufacturing equipment that manufactures the liquid to be inspected to the use point of the liquid to be inspected, and can also be separated from each other. Valves 304-1 to 304-3 are respectively equivalent to valve 304. Valves 305-1 to 305-3 are respectively equivalent to valve 305. Containers 501-1 to 501-3 that store eluents 502-1 to 502-3 are respectively equivalent to container 501. The filling container 503-1 to the filling container 503-3 are respectively equivalent to the filling container 503. The recovery container 504-1 to the recovery container 504-3 are respectively equivalent to the recovery container 504. It should be noted that the eluent 502-1 to the eluent 502-3 may be drawn from one container. In addition, the recovery container 504-1 to the recovery container 504-3 may also be one container.

[0072] The control device 702 controls valves 301-1 to 301-3, valves 304-1 to 304-3, and valves 305-1 to 305-3 in the same manner as the control device 700 in the first embodiment. The processing of the concentration process, the purge process, the eluent filling process, the elution recovery process, and the cleaning process in each system is the same as in the first embodiment. In the third embodiment, the control device 702 controls the timing of the processing of the concentration process, the purge process, the eluent filling process, the elution recovery process, and the cleaning process between each system.

[0073] Fig.13 It is used to illustrate Fig.121 is a timing chart of an example of timing control between systems performed by the control device 702 shown in FIG. In the system equipped with the concentration column 200-1 (hereinafter referred to as system A), the system equipped with the concentration column 200-2 (hereinafter referred to as system B), and the system equipped with the concentration column 200-3 (hereinafter referred to as system C), the concentration process, the purge process, the eluent filling process, the elution recovery process, and the cleaning process are sequentially repeated. At this time, the control device 702 controls so that the timing of the elution recovery process in each system in the system A, the system B, and the system C does not overlap between the systems. In addition, the control device 702 controls the valves 301-1 to 301-3, the valves 304-1 to 304-3, and the valves 305-1 to 305-3 so that the liquid to be inspected passes through the concentration column of at least one of the systems A, the system B, and the system C. That is, the control device 702 performs the control of switching the liquid flow, which controls the liquid to be inspected supplied from the ultrapure water production equipment, etc. to pass to the concentration columns 200-1 to 200-3. In this embodiment, although an example of three systems arranged in parallel is given for explanation, the number of systems is not limited thereto. Even if the recovery containers 504-1 to 504-3 are one container, by setting the timing of the recovery of each of the multiple points to different timings as described above, it is possible to perform separate analysis on each concentration column. In addition, even if the timing of the analysis or other processes overlaps, it is possible to perform separate eluent recovery by controlling the timing of the elution recovery process using the control device 702.

[0074] Thus, in this method, a plurality of systems for analyzing the liquid to be inspected at different points are arranged in parallel, and are controlled so that the timing of the elution recovery process between the systems does not overlap. Thus, the concentration process can be continuously performed, and therefore the inspection results can be continuously obtained.

[0075] Hereinafter, a method of using the above-mentioned impurity acquisition system will be described. Fig.14 This is a diagram showing an example of a liquid production and supply system to which the impurity acquisition system of the present invention is applied. Fig.14 The method shown is a system for supplying ultrapure water to a semiconductor cleaning device (use point) via a non-regenerative ion exchange device, CP1000, and an ultrafiltration device, UF1100, in an ultrapure water manufacturing device. The ultrapure water (test object water) supplied to CP1000 is supplied from a liquid manufacturing supply device installed upstream. The liquid manufacturing supply device is also a device for manufacturing ultrapure water. Fig.14 The dashed line shown indicates a flow path of water or a path of a control signal used to inspect the water quality of ultrapure water as the liquid to be inspected.

[0076] As a flow path for supplying ultrapure water to a semiconductor cleaning device, two systems are provided. An impurity removal unit 1200 is provided in one of the flow paths (systems), and ultrapure water is supplied to the semiconductor cleaning device via the impurity removal unit 1200. In addition, an on-off valve 2000 is provided between CP1000 and UF1100. In addition, an on-off valve 2300 is provided to control the flow path of water from CP1000 to the drainage line. In addition, an on-off valve 2400 is provided to control the flow path of water from UF1100 to the drainage line. In addition, an on-off valve 2100 and an on-off valve 2200 are provided in the two flow paths, respectively, and the two flow paths are used to supply ultrapure water to the semiconductor cleaning device. The water discharged from the drainage line is not only recovered to the drainage treatment equipment, but also can be recovered to the tank provided in the ultrapure water equipment.

[0077] Impurity acquisition system 1300 is equivalent to Figure 1 , Fig. 9 , Fig.13 The impurity acquisition systems shown respectively perform the processing described in the first to third embodiments on the ultrapure water from CP1000 or the ultrapure water from UF1100 as the liquid to be inspected. ICP-MS (inductively coupled plasma mass spectrometry) 1400 is a device (information processing device) for detecting the amount of impurities in the acquired eluent. The operation processing device 1600 is a device for calculating the amount (including concentration) of impurities in the liquid to be inspected, and the device performs calculations based on the cumulative flow rate obtained by the cumulative flow meter 411 of the impurity acquisition system 1300 in the concentration process and the amount of impurities in the eluent detected by the ICP-MS1400. The impurity acquisition system 1300, ICP-MS1400 and the operation processing device 1600 constitute a quality inspection system. The control device 1500 is a second control device, and controls the opening and closing of the opening and closing valves 2000, 2100, 2200, 2300, and 2400 based on the amount of impurities obtained by the quality inspection system. It should be noted that the control device 1500 can also have the functions of the above-mentioned control devices 700 to 702. The information processing device is not particularly limited as long as it is a device that can detect the amount of impurities. As an information processing device, for example, a method using ICP-MS, ICP-OES (inductively coupled plasma optical emission spectrometer), an atomic absorption spectrophotometer, an ion chromatography analyzer, etc. can be cited.

[0078] When the impurity concentration obtained by the quality inspection system for the outlet water of CP1000 exceeds the pre-set concentration threshold, the control device 1500 controls the on-off valve 2000 to be closed. At this time, the control device 1500 controls the on-off valve 2300 to be open. In addition, when the impurity concentration obtained by the quality inspection system for the outlet water of CP1000 is below the concentration threshold, the control device 1500 controls the on-off valve 2000 to be open. At this time, the control device 1500 controls the on-off valve 2300 to be closed. In addition, when the impurity concentration obtained by the quality inspection system for the outlet water of UF1100 exceeds the pre-set concentration threshold, the control device 1500 controls the on-off valve 2100 and the on-off valve 2200 to be closed. At this time, the control device 1500 controls the on-off valve 2400 to be open. In addition, when the impurity concentration obtained by the quality inspection system for the outlet water of UF1100 is below the concentration threshold, the control device 1500 controls the on-off valve 2100 and the on-off valve 2200 to be in the open state. At this time, the control device 1500 sets the on-off valve 2400 to the closed state. It should be noted that, when the impurity concentration obtained by the quality inspection system for the outlet water of UF1100 is below the first concentration threshold, the control device 1500 may also control the on-off valve 2100 to be in the open state. In addition, when the impurity concentration obtained by the quality inspection system for the outlet water of UF1100 exceeds the first concentration threshold and is below the second concentration threshold, the control device 1500 may also control the on-off valve 2200 to be in the open state and the on-off valve 2100 to be in the closed state. In addition, when the impurity concentration obtained by the quality inspection system for the outlet water of UF1100 exceeds the second concentration threshold, the control device 1500 may also control the on-off valve 2100 and the on-off valve 2200 to be in the closed state. This is because, in the flow path provided with the impurity removal unit 1200, even if the impurity concentration is high to a certain extent, the impurities contained in the ultrapure water are removed by the impurity removal unit 1200, thereby utilizing the fact that the impurity concentration of the ultrapure water supplied to the semiconductor cleaning device is reduced.

[0079] The following, Fig.14 The processing in the system shown is described. Fig.15 It is used to illustrate Fig.14 Here, the quality inspection system is used to perform a process of Fig.14The case of calculating the impurity concentration of the outlet water of UF1100 shown in FIG. 1 is described as an example. First, for the outlet water of UF1100, ICP-MS1400 detects the amount of impurities in the elution recovery liquid recovered in the recovery container 504 of the impurity acquisition system 1300 (step S31). The detection can be a method using negative pressure suction based on ICP-MS1400, or a method using gas or pumps for transportation to detect. Therefore, based on the cumulative flow rate obtained by the cumulative flowmeter 411 of the impurity acquisition system 1300 in the concentration process and the amount of impurities contained in the elution recovery liquid detected by ICP-MS1400, the operation processing unit 1600 calculates the concentration of the outlet water of UF1100 (step S32). Concentration information representing the calculated concentration is sent from the operation processing unit 1600 to the control unit 1500. The control unit 1500 determines whether the concentration represented by the sent concentration information exceeds a preset concentration threshold (step S33). When the concentration indicated by the sent concentration information exceeds the concentration threshold, the control device 1500 closes the given on-off valve (step S34). The given on-off valve is an on-off valve that prevents the ultrapure water from the ultrapure water manufacturing equipment from being supplied to the semiconductor cleaning device, for example, the on-off valve 2100 and the on-off valve 2200. At this time, the control device 1500 may also control the on-off valve 2400 to be in an open state to supply ultrapure water to the drainage pipeline. Next, the control device 1500 notifies the situation that the concentration indicated by the sent concentration information exceeds the concentration threshold (step S35). The notification is a notification to the system manager, operator, manager of the ultrapure water manufacturing equipment, etc., and is an output such as the sending of information indicating this situation and the display of a screen. Here, as described above, two thresholds for comparison with the concentration may also be set, and the control device 1500 controls the opening and closing of the on-off valve 2100 and the on-off valve 2200 based on the results of comparing the concentration with the two thresholds. The specific method of this control is as described above. In addition, for Fig.14 The outlet water of CP1000 shown is also subjected to the same processing as above when the impurity concentration is calculated by the quality inspection system.

[0080] Fig.16 FIG. 2 is a diagram showing another example of a liquid production supply system to which the impurity acquisition system of the present invention is applied. Fig.16 In the application example shown, CP1000, UF1100, impurity acquisition system 1300, ICP-MS1400, operation processing device 1600, control device 1500 and opening and closing valve 2400 are respectively Fig.14The CP1000, UF1100, impurity acquisition system 1300, ICP-MS1400, operation processing device 1600, control device 1500 and opening and closing valve 2400 shown are the same. The outlet water, i.e., ultrapure water, is distributed from UF1100 to a plurality of flow paths and supplied to a plurality of semiconductor cleaning devices connected to each flow path. A plurality of flow paths branch out into flow paths leading to the impurity acquisition system 1300, and for the ultrapure water flowing in each flow path, each ultrapure water is used as the inspection object water, and the treatment described in the first embodiment to the third embodiment is performed in the impurity acquisition system 1300. The control device 1500 controls the opening and closing of the opening and closing valves 2500-1 to 2500-4 provided in each branch flow path to select the flow path in which the ultrapure water flowing is to be processed. In addition, the control device 1500 controls the opening and closing of the opening and closing valves 2100-1 to 2100-4 provided in each flow path based on the impurity concentration obtained by the quality inspection system, similarly to the above-mentioned process. It should be noted that there may be threshold values ​​corresponding to the plurality of semiconductor cleaning devices, respectively, and the control device 1500 controls the opening and closing of the opening and closing valves 2100-1 to 2100-4 based on the comparison between the impurity concentration obtained by the quality inspection system and the threshold value.

[0081] In this way, when the concentration of impurities contained in ultrapure water exceeds a given concentration threshold, the on-off valve is controlled to prevent the supply of ultrapure water to the semiconductor cleaning device. In this way, it is possible to prevent the contamination of components in semiconductor manufacturing equipment and ultrapure water equipment. It should be noted that the liquid (water) used as the measurement object is not limited to ultrapure water, but may also be liquids such as hydrochloric acid, IPA (isopropyl alcohol), PGMA (polyglycidyl methacrylate), and PGMEA (propylene glycol monomethyl ether acetate). In addition, a method of recovering the eluent using a bottle is described, but it may also be a method of spraying the recovered eluent directly onto an analysis device for quantitative analysis. In addition, although the concentration of metal impurities measured in the present impurity acquisition system is not particularly limited, it is preferably less than 100 ng / L, more preferably less than 10 ng / L, and further preferably less than 0.1 ng / L.

[0082] In the above description, each component is assigned each function (process), but the assignment is not limited to the above assignment. In addition, regarding the structure of the component, the above mode is only an example and is not limited to this. In addition, each embodiment can also be combined.

[0083] Although the present invention has been described above with reference to the embodiments, the present invention is not limited to the above embodiments. The structure and details of the present invention can be modified in various ways that can be understood by those skilled in the art within the scope of the present invention.

[0084] This application claims the benefit of priority based on Japanese patent application No. 2022-129978, filed on August 17, 2022, the disclosure of which is incorporated herein by reference in its entirety.

Claims

1. An impurity acquisition system for acquiring impurities in a liquid to be inspected, the impurity acquisition system comprising: A first adsorber that adsorbs impurities in the liquid to be inspected; and A first control device switches between a concentration process, an eluent filling process and an elution recovery process. In the concentration process, the liquid to be inspected is passed to the first adsorbent. In the eluent filling process, a given amount of eluent is filled into a filling container, and the eluent elutes impurities adsorbed on the first adsorbent. In the elution recovery process, the eluent filled in the filling container is passed to the first adsorbent and recovered to a recovery container.

2. The impurity acquisition system according to claim 1, wherein: The first control device performs a purge process after the concentration process. In the purge process, gas is injected into the liquid passage of the liquid to be inspected and the first adsorbent to perform purge.

3. The impurity acquisition system according to claim 1 or 2, wherein: The first control device causes the eluent to flow in the elution recovery step in a direction opposite to the direction in which the liquid to be inspected flows toward the first adsorbent in the concentration step.

4. The impurity acquisition system according to claim 1 or 2, wherein: The first control device performs a cleaning process after the elution recovery process. In the cleaning process, a cleaning liquid for cleaning the first adsorbent is passed into the first adsorbent.

5. The impurity acquisition system according to claim 4, wherein: The first control device performs a regeneration process after performing the cleaning process as the first cleaning process, and performs a second cleaning process after performing the regeneration process. In the regeneration process, the regeneration liquid for regenerating the first adsorbent body is passed into the first adsorbent body, and in the second cleaning process, the cleaning liquid is passed into the first adsorbent body.

6. The impurity acquisition system according to claim 5, wherein: The first control device causes the regeneration liquid to flow in the regeneration step in a direction opposite to the direction in which the liquid to be inspected is passed to the first adsorbent in the concentration step.

7. The impurity acquisition system according to claim 5, wherein: In the first cleaning step and the second cleaning step, the first control device supplies liquid obtained by passing the liquid to be inspected through a second adsorption body that adsorbs impurities in the liquid to be inspected as the cleaning liquid to the first adsorption body.

8. The impurity acquisition system according to claim 1 or 2, wherein: The impurity acquisition system is provided with: A plurality of acquisition units, for respectively acquiring the liquid to be inspected from a plurality of points on a path from a device for manufacturing the liquid to be inspected to a point of use of the liquid to be inspected; as well as The plurality of first adsorbents are for the liquids obtained from the plurality of points by using the plurality of obtaining units to pass through respectively. The first control device performs a plurality of elution recovery steps for each of the plurality of first adsorbents at timings that do not overlap with each other.

9. A quality inspection system comprising: The impurity acquisition system according to claim 1 or 2; an information processing device for detecting the amount of impurities in the eluted recovery liquid after passing through the first adsorber; and An operation processing device calculates the amount of impurities in the liquid to be inspected.

10. A liquid manufacturing supply system, comprising: The quality inspection system according to claim 9; a valve portion that controls supply of the liquid to be inspected from a liquid manufacturing and supplying device that performs at least one of manufacturing and supplying the liquid to be inspected to a use point that uses the liquid to be inspected; and A second control device controls the valve portion based on the amount of foreign matter in the liquid to be inspected calculated by the arithmetic processing device.

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