JP6981443B2 - Online measurement method of liquid component concentration - Google Patents

Description

The present invention relates to an online method for measuring a liquid component concentration.

Conventionally, a densitometer is installed in a tank that stores a treatment liquid used online, and a stock solution is added to the tank according to the fluctuation of the concentration of a specific component of the treatment liquid in the tank detected by the densitometer. There are known methods such as increasing the concentration or adding a solvent to dilute the concentration. However, in this conventional method, the concentration deviation in the treatment liquid is large depending on the measurement position of the concentration in the tank, and the difference between the concentration of the treatment liquid actually used online and the measured concentration. May increase.

In Patent Document 1, the cooling water supplied to the level setting container via the test fluid supply pipe branched from the main stream main to which the cooling water of the cooling device for cooling the manufacturing equipment flows is applied to the bottom of the level setting container. It flows down in a columnar shape from a provided nozzle, irradiates the columnar cooling water with light having a specific wavelength, detects the amount of fluorescence of the fluorescence emitted by the specific component in the coolant, and detects the specific component in the coolant. A concentration measuring method for continuously measuring the concentration of water is disclosed. As a result, the concentration of the specific component in the coolant can be continuously measured online, and the difference between the concentration in the coolant actually used online and the measured concentration becomes large. Can be suppressed.

Japanese Unexamined Patent Publication No. 2008-39685

However, since the concentration measuring method disclosed in Patent Document 1 is premised on continuously measuring the concentration of a specific component in a liquid online, when different products that do not use a treatment liquid are manufactured in the same equipment. In addition, when the concentration of the treatment liquid is measured intermittently as in the case of line stop, there are problems such as sticking or clogging of the solution and deterioration of the concentration measurement accuracy.

The present invention has been made in view of the above problems, and an object thereof is that even when the concentration of a treatment liquid is intermittently measured online, the solution may be stuck or clogged, or the concentration measurement accuracy may be lowered. It is an object of the present invention to provide an online method for measuring a liquid component concentration capable of suitably measuring the concentration of a specific component of a treatment liquid without any trouble.

To solve the above problems and achieve the object, on-line measurement method of the liquid component density of the present invention supplies a process liquid from the process liquid circulation tank to the online tank, using the processing solution in the online operation during, and supplied to the measurement apparatus from the processing solution circulating tank via a pipe the treatment liquid online, it is possible to measure the concentration of a specific component of the treatment liquid by the measuring device, and the at-line When it is necessary to stop the measurement of the concentration by the measuring device after the operation using the treatment liquid is finished, the supply of the treatment liquid to the measuring device is stopped and the piping to the measuring device is stopped. It is characterized in that a cleaning liquid is supplied from a cleaning liquid supply facility via a cleaning liquid supply facility, the measuring device and the piping are cleaned, and the cleaning liquid after cleaning the measuring device and the piping is discharged to a waste liquid tank. be.

Further, in the method for measuring the liquid component concentration according to the present invention, in the above invention, a part of the treated liquid supplied via the pipe is overflowed to keep the liquid level of the treated liquid at the same level. The flow rate when the treatment liquid is made to flow down from the bottom of the level setting container, the treatment liquid is supplied to the measuring device, and the treatment liquid is supplied to the level setting container, is adjusted by a flow rate provided in the pipe. It is characterized by being regulated by a valve.

Further, in the above-mentioned invention, the online measuring method of the liquid component concentration according to the present invention is described from the level setting container when the concentration of the treated liquid supplied to the measuring device from the level setting container is measured by the measuring device. It is characterized in that the supply of the processing liquid to the measuring device is stopped.

The online method for measuring the concentration of a liquid component according to the present invention treats the solution without causing sticking or clogging of the solution or deteriorating the concentration measurement accuracy even when the concentration of the treated liquid is intermittently measured online. It has the effect that it is possible to suitably measure the concentration of a specific component of the liquid.

FIG. 1 is a diagram showing a piping system according to an embodiment. FIG. 2 is a flowchart showing an example of control of online tank operation processing in the embodiment. FIG. 3 is a flowchart showing an example of control of the analyzer operation process in the embodiment. FIG. 4 is a flowchart showing an example of control of the operation stop process and the cleaning process in the embodiment.

Hereinafter, an embodiment of the online measurement method for the liquid component concentration according to the present invention will be described. The present invention is not limited to the present embodiment.

FIG. 1 is a diagram showing a piping system according to an embodiment. As shown in FIG. 1, in the piping system according to the present embodiment, the chemical solution is supplied from the piping 100 connected to the chemical solution circulation tank 1 to the piping 102 for sending the chemical solution to the online tank 3 side and the analyzer 9 side. It is branched into a pipe 202 for sending. The chemical liquid circulation tank 1 is installed offline and stores the chemical liquid which is a treatment liquid used online. The online tank 3 is installed online, and temporarily stores, for example, a chemical solution supplied to a coating device (not shown) that applies the chemical solution to a product split (not shown) online. For example, in the case of spray painting, the residual chemical solution after spray painting on the product is temporarily stored. The analyzer 9 can measure (analyze) the concentration of a specific component of the sample solution in real time by using the drug solution having the same component as the drug solution supplied online from the drug solution circulation tank 1 to the online tank 3 as the sample solution. Functions as a measuring device. The pipe 100 is provided with a shutoff valve 10 for allowing or shutting off the flow of liquid to the pipe 102 and the pipe 202.

Two pipes 104a and 104b are connected to the online tank 3 for branching from the pipe 102 and supplying the liquid to the online tank 3. For example, in the case of spray painting in the online tank 3, the chemicals supplied from the pipes 104a and 104b are coated on the front and back surfaces, and the residual chemicals are temporarily stored in the online tank 3. The pipe 102 is provided with a pump 41 which is a power source for sending liquid and a shutoff valve 12. The shutoff valve 12 is located on the downstream side of the pump 41 and on the upstream side of the branch point between the two pipes 104a and 104b.

Further, a pipe 106 for discharging the liquid from the online tank 3 is connected to the online tank 3, a pipe 108 branched from the pipe 106 is connected to the chemical liquid circulation tank 1, and a pipe 110 branched from the pipe 106 is connected. It is connected to the waste liquid tank 50. The pipe 106 is provided with a shutoff valve 14 for allowing or shutting off the flow of liquid from the online tank 3 to the chemical liquid circulation tank 1. Further, the pipe 110 is provided with a shutoff valve 16 for allowing or shutting off the flow of liquid from the online tank 3 to the waste liquid tank 50.

For the supply of the sample liquid from the chemical liquid circulation tank 1 to the analyzer 9, a level setting container 5 that overflows a part of the sample liquid supplied through the pipe 202 and keeps the liquid level of the sample liquid at the same level is provided. It is done through. An ultrasonic level meter 7 for measuring the liquid level (liquid amount) in the level setting container 5 is attached to the level setting container 5. The downstream side piping portion 202a in the piping 202 is connected to the level setting container 5. The pipe 202 is provided with a pump 42, which is a power source for sending liquid, and a flow rate control valve 20. The flow rate control valve 20 is arranged on the downstream side of the pump 42, and the flow rate of the liquid supplied to the level setting container 5 can be adjusted by changing the opening degree. The downstream piping portion 202a refers to a portion of the piping 202 between the flow rate control valve 20 and the level setting container 5.

In the present embodiment, the flow rate of the liquid supplied to the level setting container 5 can be adjusted by the flow rate control valve 20. This makes it possible, for example, to prevent the sample liquid from being ruffled or bubbling in the level setting container 5 when the sample liquid is supplied to the level setting container 5. Therefore, the liquid level of the sample liquid in the level setting container 5 can be remotely monitored by the ultrasonic level meter 7, and it can be confirmed that the sample liquid is retained in the level setting container 5.

Considering the amount of the sample liquid used in the analyzer 9, the level setting container 5 is preferably a container having a capacity of about 21 [L] to 30 [L]. Therefore, as a level meter for monitoring the liquid level of the sample liquid in the level setting container 5, a differential pressure transmitter type, an electrode type, or a guide pulse type level meter, which is premised on measurement in a large tank, is a level. It is difficult to monitor the liquid level (liquid amount) in the setting container 5. Further, in the present embodiment, since the structure is such that the liquid is drained from the lower surface of the level setting container 5, it is difficult to monitor the liquid level (liquid amount) in the level setting container 5 even with a load measuring type level meter. Therefore, in the present embodiment, the ultrasonic level meter 7 is used to monitor the liquid level (liquid amount) in the level setting container 5.

When the liquid level (liquid amount) in the level setting container 5 exceeds a certain level, the sample liquid overflows from the level setting container 5, the sample liquid flows into the pipe 206, and the pipe 206, the pipe 210, and the pipe 212 are used. The liquid is sent to the chemical liquid circulation tank 1 through the above. Therefore, the liquid level (liquid amount) of the sample liquid in the level setting container 5 can be stabilized without the need to control the liquid level by only monitoring with the ultrasonic level meter 7.

Further, in the present embodiment, on the premise that the downstream piping portion 202a for sending the liquid to the level setting container 5 is a flow path that does not flow back from the level setting container 5, the level setting container 5 causes an overflow. It is connected to the level setting container 5 at a position below the liquid level. As a result, it is possible to obtain a relatively gentle liquid level in which waviness and bubbling in the level setting container 5 are suppressed, and the sample liquid in the level setting container 5 is stirred, and the same sample liquid remains retained. It can be made difficult.

The level setting container 5 and the analyzer 9 are connected by a pipe 204. The pipe 204 is provided with a flow rate control valve 21 and a shutoff valve 22. The flow rate control valve 21 can adjust the flow rate of the liquid supplied from the level setting container 5 to the analyzer 9 by changing the opening degree. The shutoff valve 22 allows or shuts off the flow of liquid from the level setting container 5 to the analyzer 9.

In the present embodiment, the sample liquid in the level setting container 5 has an appropriate height h from the upper end of the analyzer 9 to the lower end of the level setting container 5 at a substantially stable pressure required and sufficient by the analyzer 9. Can flow down to the analyzer 9. Furthermore, by setting the opening degree of the flow rate control valve 21 in advance, it is possible to adjust the flow rate of the sample liquid supplied from the level setting container 5 to the analyzer 9, and the analyzer 9 is a laboratory specification. However, the burden can be reduced and the sample liquid can be supplied to the analyzer 9.

Further, in the present embodiment, since the shutoff valve 22 is provided on the lower surface of the level setting container 5 and the pipe 204 connected to the analyzer 9, the level can be set by automatically and remotely controlling the opening and closing of the shutoff valve 22. It is possible to automatically instruct the timing of supplying the sample liquid from the container 5 to the analyzer 9.

A pipe 206 for circulating the liquid overflowing from the level setting container 5 is connected to the level setting container 5. A pipe 208 branched from the pipe 204 is connected to the middle of the pipe 206 on the upstream side of the flow rate control valve 21. The pipe 208 is provided with a shutoff valve 23 for allowing or shutting off the flow of the liquid from the level setting container 5 through the pipe 204 and the pipe 208 to the pipe 206.

Thereby, in the present embodiment, by opening the shutoff valve 23, the sample liquid in the level setting container 5 can be discharged to the pipe 206 through the pipe 204 and the pipe 208. Therefore, it is possible to store the sample liquid in the level setting container 5 again and shorten the operation time until the next analysis by the analyzer 9 is started.

Further, a pipe 210 for discharging the liquid from the analyzer 9 is connected to the analyzer 9, a pipe 212 branched from the pipe 210 is connected to the chemical liquid circulation tank 1, and a pipe 214 branched from the pipe 210 is connected. It is connected to the waste liquid tank 50. The pipe 210 is provided with a shutoff valve 24 for allowing or shutting off the flow of liquid from the analyzer 9. The pipe 212 is provided with a shutoff valve 25 for allowing or shutting off the flow of liquid from the pipe 210 to the chemical liquid circulation tank 1. The pipe 214 is provided with a shutoff valve 26 for allowing or shutting off the flow of liquid from the pipe 210 to the waste liquid tank 50. Further, the pipe 206 is connected to the pipe 210 on the downstream side of the shutoff valve 24 and on the upstream side of the branch point of the pipe 212 and the pipe 214.

In the present embodiment, the shutoff valve 24 is provided in the pipe 210 connected to the analyzer 9, and the opening / closing operation of the shutoff valve 22 and the shutoff valve 24 can be automatically remotely controlled and linked. .. As a result, the shutoff valve 22 is opened, the shutoff valve 24 is closed, the sample liquid is sent from the level setting container 5 to the analyzer 9, and then the shutoff valve 22 is closed to stop the flow of the sample liquid in the analyzer 9. It is possible and stable analysis can be performed. Further, in the present embodiment, after the analysis by the analyzer 9 is completed, the shutoff valve 24 is opened to discharge the sample liquid in the analyzer 9 to the pipe 210, and when the discharge of the sample liquid from the analyzer 9 is completed. It is possible to close the shutoff valve 24 and open the shutoff valve 22 to supply the sample liquid from the level setting container 5 to the analyzer 9. As described above, in the present embodiment, the opening / closing operation of the shutoff valve 22 and the shutoff valve 24 is automatically remotely controlled and linked to repeatedly supply and discharge the sample liquid to the analyzer 9, and the level setting container. Since the same sample solution retained in 5 can be supplied to the analyzer 9 in a plurality of times and the analysis can be repeated, variations in the analytical values can be reduced and stable analysis results can be obtained. ..

Further, a pipe 302 connected to the washing water supply facility 62 is connected to the pipe 202 on the upstream side of the pump 42 and on the downstream side of the branch point with the pipe 102. The pipe 302 is provided with a shutoff valve 32 for allowing or shutting off the flow of wash water from the wash water supply facility 62 to the pipe 202.

Here, in the present embodiment, after the online operation using the chemical solution is completed, for example, the surface treatment of the product split using the chemical solution stored in the online tank 3 is completed, and the chemical solution circulation tank 1 and the online tank 3 are completed. After stopping the circulation of the chemical solution to and from, it is possible to perform cleaning of the online tank 3, the level setting container 5, the analyzer 9, and each pipe using the above-mentioned piping system. ing.

When it is necessary to stop the concentration measurement by the analyzer 9 after the operation using the chemical solution online is completed, first, the pump 41 and the pump 42 are stopped, the shutoff valve 10 is closed, and the chemical solution circulation tank 1 is stopped. The supply of the chemical solution and the sample solution to the online tank 3 and the level setting container 5 is stopped. After that, the chemical solution in the online tank 3 and the sample solution in the level setting container 5 are discharged, and the chemical solution and the sample solution are waited to be returned from the online tank 3 and the level setting container 5 to the chemical solution circulation tank 1. At this time, by opening the shutoff valve 23, the sample liquid can be discharged from the level setting container 5 through the pipe 208. Therefore, the discharge of the sample liquid from the level setting container 5 can be made faster than the case where the sample liquid is simply discharged from the level setting container 5 via the analyzer 9.

After the discharge of the chemical solution and the sample solution from the online tank 3 and the level setting container 5 is completed, the shutoff valve 32 is opened and the washing water supply facility 62 is connected to the pipe 102 on the online tank 3 side and the pipe 202 on the level setting container 5. The wash water consisting of pure water is discharged. At this time, whether to restart or not restart the pump 41 and the pump 42 depends on the level of the pressure of the washing water. The washing water sent from the washing water supply facility 62 to the pipe 102 flows into the pipe 110 via the online tank 3. At this time, since the washing water cannot be reused as a chemical solution, the washing water can be dumped into the waste liquid tank 50 by automatically closing the shutoff valve 14 and opening the shutoff valve 16 by remote control.

The washing water sent from the washing water supply facility 62 to the pipe 202 cleans the pipe 202 and the flow control valve 20, and subsequently cleans the level setting container 5. When cleaning the level setting container 5, unlike the sample liquid, it is desired to pour the washing water into the level setting container 5 with a little vigor. Therefore, by setting the opening degree of the flow rate control valve 20 to a different opening degree from that in the analysis process, the flow rate of the washing water to the level setting container 5 at the time of washing is automatically changed. If a certain amount of wash water is accumulated in the level setting container 5 and the cleanliness of the wash water is insufficient, the shutoff valve 23 is intermittently opened and closed a plurality of times to enter the level setting container 5. It is possible to promote the cleaning of the cleaning water and increase the cleanliness of the cleaning water.

Further, it is sufficient to supply the washing water into the level setting container 5 with the shutoff valve 23 closed and leave the washing water in the level setting container 5 for a certain period of time so that the washing water overflows from the level setting container 5. After a lapse of time, the shutoff valve 22 and the shutoff valve 24 are opened. As a result, the washing water can be sent from the level setting container 5 to the analyzer 9 at the timing when a sufficient amount of water is secured for cleaning the analyzer 9. At this time, the flow rate of the washing water from the level setting container 5 to the analyzer 9 is set by setting the opening degree of the flow control valve 21 within a range that does not impose a burden on the analyzer 9. The amount of water that allows sufficient washing water to pass through can be automatically changed.

After the cleaning of the level setting container 5 and the analyzer 9 is completed, the shutoff valve 23 is opened and the shutoff valve 22 and the shutoff valve 24 are closed to completely drain the washing water in the level setting container 5. Considering that a small amount of the chemical solution component remains in the analyzer 9, the effect of delaying drying and solidification can be obtained. Further, the washing water in the analyzer 9 is not returned to the chemical liquid circulation tank 1, but is automatically discharged to the waste liquid tank 50 through the pipe 210 and the pipe 214.

Further, in the present embodiment, the chemical liquid circulation tank 1 is connected to the pipe 304 connected to the pure water supply facility 64. The pipe 304 is provided with a shutoff valve 34 for allowing or shutting off the flow of pure water from the pure water supply facility 64 to the chemical liquid circulation tank 1. Further, a pipe 306 connected to the stock solution supply facility 66 is connected to the chemical liquid circulation tank 1. The pipe 306 is provided with a shutoff valve 36 for allowing or shutting off the flow of the undiluted solution from the undiluted solution supply facility 66 to the chemical liquid circulation tank 1.

In the present embodiment, as a result of analysis by the analyzer 9, pure water is additionally supplied from the shutoff valve 34 to the chemical liquid circulation tank 1 in order to dilute if the drug concentration is high, and if the drug concentration is low, the shutoff valve 36 is used to increase the concentration. The undiluted solution is additionally supplied to the chemical solution circulation tank 1. However, the amount of pure water or undiluted solution added to the chemical liquid circulation tank 1 is calculated based on the liquid amount of the chemical liquid circulation tank 1 and the measurement result of the analyzer 9. Further, after the pure or undiluted solution is additionally supplied to the chemical solution circulation tank 1, the drug concentration in the chemical solution circulation tank 1 is made uniform with sufficient stirring.

In this embodiment, various operations such as opening / closing operation of each shutoff valve, setting of opening degree of each flow rate control valve, operation / stop of each pump, and concentration measurement by the analyzer 9 are not shown. It is automatically performed by remote control by the control device.

FIG. 2 is a flowchart showing an example of control of online tank operation processing in the embodiment. Here, the process of circulating the chemical solution between the chemical solution circulation tank 1 and the online tank 3 during the operation using the chemical solution online is referred to as an online tank operation process.

As shown in FIG. 2, in the control of the online tank operation process, the control device first creates an initial state (step S1). Next, the control device opens the shutoff valve 10 (step S2). As a result, the distribution of the chemical solution from the chemical solution circulation tank 1 to the pipe 102 is allowed. Next, the control device opens the shutoff valve 12 (step S3). As a result, the distribution of the chemical solution from the pipe 102 to the pipes 104a, 104b and, by extension, the online tank 3 is permitted. Next, the control device opens the shutoff valve 14 (step S4). As a result, the distribution of the chemical liquid from the pipe 106 connected to the online tank 3 to the pipe 108 and eventually to the chemical liquid circulation tank 1 is permitted. At this time, the shutoff valve 16 provided in the pipe 110 is closed, and the flow of the chemical liquid from the online tank 3 through the pipe 106 and the pipe 110 to the waste liquid tank 50 is cut off by the shutoff valve 16. .. Next, the control device operates the pump 41 (step S5). As a result, the chemical liquid is sent from the chemical liquid circulation tank 1 to the online tank 3 through the pipe 100, the pipe 102, and the pipes 104a and 104b by the power of the pump 41. At the same time, the chemical liquid is sent from the online tank 3 to the chemical liquid circulation tank 1 through the pipe 106 and the pipe 108. In this way, in the present embodiment, the chemical solution is circulated between the chemical solution circulation tank 1 and the online tank 3. Next, the control device determines whether the operation using the chemical solution is completed online and the operation of the online tank 3 is stopped (step S6). If it is determined that the operation is not stopped (No in step S6), the control device repeatedly executes the process of step S6 until it is determined that the operation is stopped. On the other hand, when it is determined that the operation is stopped (Yes in step S6), the control device ends a series of controls and controls the operation stop process and the cleaning process, which will be described later.

FIG. 3 is a flowchart showing an example of control of the analyzer operation process in the embodiment. Here, a process of circulating a sample liquid (chemical liquid) between the chemical liquid circulation tank 1 and the analyzer 9 and analyzing (measuring) the concentration of a specific component of the sample liquid by the analyzer 9 is performed by the analyzer. Let's call it operation processing.

As shown in FIG. 3, in the control of the analyzer operation process, the control device first creates an initial state (S101). Next, the control device closes the shutoff valve 22 and the shutoff valve 24 (step S102). As a result, the flow of the sample liquid from the pipe 204 connected to the level setting container 5 to the analyzer 9 is blocked by the shutoff valve 22. Further, the flow of the sample liquid from the analyzer 9 to the pipe 210 is cut off by the shutoff valve 24. Next, the control device sets the opening degree of the flow rate control valve 20 (step S103). The opening degree of the flow rate control valve 20 at this time is set so that the sample liquid is sent to the level setting container 5 at a flow rate that does not cause the sample liquid to undulate or foam in the level setting container 5, for example. do. Next, the control device closes the shutoff valve 26 (step 104). As a result, the flow of the sample liquid to the waste liquid tank 50 through the pipe 206, the pipe 210, and the pipe 214 is cut off by the shutoff valve 26 due to overflow from the level setting container 5. Next, the control device opens the shutoff valve 25 (step S105). As a result, the sample liquid is allowed to flow to the chemical liquid circulation tank 1 through the pipe 206, the pipe 210, and the pipe 212, such as overflowing from the level setting container 5. Next, the control device operates the pump 42 (step S106). As a result, the sample liquid is sent from the chemical liquid circulation tank 1 to the level setting container 5 through the pipe 100 and the pipe 202 by the power of the pump 42. At the same time, the sample liquid overflowing from the level setting container 5 is sent to the chemical liquid circulation tank 1 through the pipe 206, the pipe 210, and the pipe 212.

Next, the control device sets the opening degree of the flow rate control valve 21 (step S107). As a result, the flow rate of the sample liquid sent from the level setting container 5 to the analyzer 9 is adjusted in advance. Next, the control device opens the shutoff valve 22 (step S108). As a result, the flow of the sample liquid from the level setting container 5 to the analyzer 9 through the pipe 204 is allowed. Next, the control device opens the shutoff valve 24 (step S109). As a result, the flow of the sample liquid from the analyzer 9 through the pipe 210 and the pipe 212 to the chemical liquid circulation tank 1 is allowed. That is, at this time, the sample liquid is continuously passed from the level setting container 5 to the analyzer 9 without retaining the sample liquid in the analyzer 9.

Next, the control device closes the shutoff valve 24 (step S110). As a result, the flow of the sample liquid from the analyzer 9 through the pipe 210 and the pipe 212 to the chemical liquid circulation tank 1 is cut off by the shutoff valve 24. Therefore, the sample liquid sent from the level setting container 5 to the analyzer 9 through the pipe 204 is retained in the analyzer 9 for analysis. Next, the control device closes the shutoff valve 22 (step S111). As a result, the flow of the sample liquid from the level setting container 5 to the analyzer 9 through the pipe 204 is blocked by the shutoff valve 22.

Next, the control device starts the analysis in the analyzer 9 (step S112). As a result, the measurement (analysis) of the concentration of the specific component of the sample solution is started using the sample solution retained in the analyzer 9. Next, the control device completes the analysis in the analyzer 9 (step S113). This completes the measurement (analysis) of the concentration of the specific component of the sample liquid in the analyzer 9.

Next, the control device determines whether the iterative analysis is completed (step S114). If it is determined that the iterative analysis is not completed (No in step S114), the control device repeatedly executes the process of step S114 until it is determined that the iterative analysis is completed. On the other hand, when it is determined that the repeated analysis is completed (Yes in step S114), the control device opens the shutoff valve 23 (step S115). As a result, the flow of the sample liquid from the level setting container 5 through the pipe 204 and the pipe 208 to the pipe 206 and eventually to the chemical liquid circulation tank 1 is allowed. Therefore, the sample liquid in the level setting container 5 flows into the pipe 206 for flowing the sample liquid overflowing from the level setting container 5 through the pipe 208 branched from the pipe 204 connected to the level setting container 5. The liquid is sent to the chemical liquid circulation tank 1 through the pipe 206, the pipe 210, and the pipe 212.

Next, the control device closes the shutoff valve 23 (step S116). As a result, after the sample liquid has been sent from the level setting container 5 to the chemical liquid circulation tank 1 through the pipe 208 or the like, the shutoff valve 23 is closed to block the flow of the sample liquid in the pipe 208, and the level setting container 5 is used. Stop draining the sample liquid from. Next, the control device determines whether the operation using the chemical solution is completed online and the operation of the analyzer 9 is stopped (step S117). When it is determined that the operation is not stopped (No in step S117), the control device returns to the process of step S108 and prepares for the next analysis of the sample liquid by the analyzer 9. On the other hand, when it is determined that the operation is stopped (Yes in step S117), the control device ends a series of controls and controls the operation stop process and the cleaning process, which will be described later.

FIG. 4 is a flowchart showing an example of control of the operation stop process and the cleaning process in the embodiment. As shown in FIG. 4, in the control of the operation stop process and the cleaning process, the control device first stops the pump 41 (step S201). As a result, the power of the pump 41 stops the feeding of the chemical solution from the chemical solution circulation tank 1 to the online tank 3 side. Next, the control device stops the pump 42 (step S202). As a result, the feeding of the sample liquid from the chemical liquid circulation tank 1 to the level setting container 5 side (analyzer 9 side) by the power of the pump 42 is stopped.

Next, the control device closes the shutoff valve 10 (step S203). As a result, the flow of the chemical liquid and the sample liquid from the chemical liquid circulation tank 1 through the pipe 100 to the pipe 102 on the online tank 3 side and the pipe 202 on the level setting container 5 side (analyzer 9 side) is blocked by the shutoff valve 10. Will be done. Next, the control device holds the shutoff valve 14 in an open state (step S204). As a result, the state in which the flow of the chemical solution from the online tank 3 to the chemical solution circulation tank 1 is permitted through the pipe 106 and the pipe 108 is maintained, and the chemical solution remaining in the online tank 3 is returned to the chemical solution circulation tank 1. Next, the control device holds the shutoff valve 25 in an open state (step S205). As a result, the level setting container 5 and the analyzer 9 are maintained in a state in which the sample liquid is allowed to flow from the level setting container 5 and the analyzer 9 to the chemical liquid circulation tank 1 through the pipe 210 and the pipe 212. It is possible to return the sample liquid remaining in the chemical liquid circulation tank 1 to the chemical liquid circulation tank 1. Next, the control device sets the opening degree of the flow rate control valve 20 (step S206). Next, the control device sets the opening degree of the flow rate control valve 21 (step S207).

Next, the control device closes the shutoff valve 22 (step S208). As a result, the flow of the liquid from the level setting container 5 to the analyzer 9 through the pipe 204 is cut off by the shutoff valve 22. Next, the control device opens the shutoff valve 24 (step S209). As a result, the flow of the liquid from the analyzer 9 to the pipe 210 is allowed. Next, the control device keeps the shutoff valve 23 closed (step S210). As a result, the shutoff valve 23 is closed to shut off the flow of the liquid in the pipe 208, and the state in which the discharge of the sample liquid from the level setting container 5 is stopped is maintained.

Next, the control device keeps the shutoff valve 12 open (step S211). As a result, the state in which the flow of the liquid through the pipe 102 to the pipes 104a and 104b and, by extension, the online tank 3 is permitted is maintained. Next, the control device closes the shutoff valve 14 (step S212). As a result, the flow of the liquid from the online tank 3 through the pipe 106 and the pipe 108 to the chemical liquid circulation tank 1 is cut off by the shutoff valve 14.

Next, the control device closes the shutoff valve 25 (step S213). As a result, the flow of the liquid from the level setting container 5 and the analyzer 9 to the chemical liquid circulation tank 1 through the pipe 210 and the pipe 212 is cut off by the shutoff valve 25. Next, the control device opens the shutoff valve 26 (step S214). As a result, the flow of liquid from the level setting container 5 and the analyzer 9 to the waste liquid tank 50 through the pipe 210, the pipe 214, and the like is allowed. Next, the shutoff valve 16 is opened (step S215). As a result, the flow of the liquid from the online tank 3 through the pipe 106 and the pipe 110 to the waste liquid tank 50 is allowed.

Next, the control device opens the shutoff valve 32 (step S216). As a result, the flow of washing water from the washing water supply facility 62 through the pipe 302 to the pipe 102 on the online tank 3 side and the pipe 202 on the level setting container 5 side (analyzer 9 side) is allowed. Next, the control device opens the shutoff valve 22 (step S217). As a result, the flow of wash water from the level setting container 5 to the analyzer 9 through the pipe 204 is allowed. In this way, the washing water is supplied from the washing water supply facility 62 to the online tank 3 side via the pipe 102, and the washing water is supplied to the level setting container 5 side (analyzer 9 side) via the pipe 202. By doing so, the online tank 3, the level setting container 5, the analyzer 9, and each pipe are cleaned (step S218).

Next, the control device closes the shutoff valve 32 (step S219). As a result, the flow of washing water from the washing water supply facility 62 through the pipe 302 to the pipe 102 on the online tank 3 side and the pipe 202 on the level setting container 5 side (analyzer 9 side) is cut off by the shutoff valve 32.

Next, the control device opens the shutoff valve 23 (step S220). As a result, the flow of the washing water from the level setting container 5 through the pipe 204 and the pipe 208 to the pipe 206 and eventually to the waste liquid tank 50 is allowed. Therefore, the washing water in the level setting container 5 flows into the pipe 206 for flowing the sample liquid overflowing from the level setting container 5 through the pipe 208 branched from the pipe 204 connected to the level setting container 5. It is discharged to the waste liquid tank 50 through the pipe 206, the pipe 210, and the pipe 214. Next, the control device closes the shutoff valve 23 (step S221). As a result, after the discharge of the washing water from the level setting container 5 to the waste liquid tank 50 through the pipe 208 or the like is completed, the shutoff valve 23 is closed to shut off the flow of the washing water in the pipe 208, and the level setting container 5 is used. Stop the drainage of wash water. Next, the control device closes the shutoff valve 12 (step S222). As a result, the flow of the washing water from the pipe 102 to the pipes 104a and 104b and eventually to the online tank 3 is cut off by the shutoff valve 12.

Next, the control device closes and closes the flow rate control valve 20 (step S223). As a result, the flow of the washing water from the pipe 202 to the level setting container 5 is cut off by the flow rate control valve 20. Next, the control device closes and closes the flow rate control valve 21 (step S224). Further, the control device closes the shutoff valve 22 (step S225). As a result, the flow of the washing water from the level setting container 5 to the analyzer 9 through the pipe 204 is cut off by the flow rate control valve 21 and the shutoff valve 22. Next, the control device closes the shutoff valve 24 (step S226). As a result, the flow of the washing water from the analyzer 9 to the waste liquid tank 50 through the pipe 210 and the pipe 214 is cut off by the shutoff valve 24, and the control device ends a series of controls.

1 Chemical circulation tank 3 Online tank 5 Level setting container 7 Ultrasonic level meter 9 Analyzer 10, 12, 14, 16 Shutoff valve 20, 21 Flow control valve 22, 23, 24, 25, 26 Shutoff valve 32, 34, 36 Shutoff valve 41, 42 Pump 50 Waste liquid tank 62 Washing water supply equipment 64 Pure water supply equipment 66 Undiluted solution supply equipment 100, 102, 104a, 104b, 106, 108, 110 Piping 202, 204, 206, 208, 210, 212, 214 Piping 302, 304, 306 Piping

Claims (3)

Supplying a process liquid from the process liquid circulation tank to online tank, during operation using the treatment liquid in the line, and supplied to the measurement apparatus from the processing solution circulating tank via a pipe the treatment liquid online, the When it is possible to measure the concentration of a specific component of the treatment liquid by the measuring device and it is necessary to stop the measurement of the concentration by the measuring device after the operation using the treatment liquid is completed online. is configured to stop the supply of the treatment liquid to the measuring device, wherein the through piping cleaning liquid is supplied from the cleaning liquid supply system to the measuring device, and a cleaning of the measuring device and the pipe, said measuring device An online method for measuring a liquid component concentration, which comprises discharging the cleaning liquid after cleaning the pipe to a waste liquid tank. In the online measurement method for the liquid component concentration according to claim 1,
The treatment liquid is allowed to flow down from the bottom of the level setting container that overflows a part of the treatment liquid supplied through the pipe to keep the liquid level of the treatment liquid at the same level, and causes the measuring device to flow the treatment liquid. Supply the treatment liquid,
An online method for measuring a liquid component concentration, which comprises adjusting the flow rate when supplying the treatment liquid to the level setting container by a flow rate control valve provided in the pipe. In the method for measuring the liquid component concentration according to claim 2,
Liquid component concentration characterized by stopping the supply of the treatment liquid from the level setting container to the measuring device when the concentration of the treatment liquid supplied from the level setting container to the measuring device is measured by the measuring device. Online measurement method.

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