Refining apparatus and method for controlling the refining apparatus

JP7652298B2Active Publication Date: 2025-03-27SHIMADZU SEISAKUSHO LTD
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Patent Information

Application Number
JP2023570677
Authority / Receiving Office
JP · JP
Patent Type
Patents
Current Assignee / Owner
Priority Date
2021-12-28
Filing Date
2022-10-26
Publication Date
2025-03-27
Estimated Expiration
2042-10-26

AI Technical Summary

Benefits of technology

【0007】 本開示による精製装置によれば、容器に対して第1導入と後続の第2導入を含む複数回の分解液の導入が行なわれ、後の導入ほど分解液中に含まれる分解物質の量が多くなる。これにより、試料中に未分解の夾雑物が多く含まれている第1導入においては、比較的少ない量の分解物質により、穏やかに分解を行なうことができる。そして、未分解の夾雑物が少なくなった状態で、第1導入より多量の分解物質を加えることで、残った夾雑物を確実に分解することができる。したがって、分解液による分解を適切に完了し、混合試料中の夾雑物の残留を低減することができる。

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Abstract

A refining device according to the present invention refines a sample and comprises a container and a control device. The container accommodates the sample and introduces a decomposing liquid containing decomposing substances for decomposing contaminants in the sample. The control device controls the container so as to introduce a multiple-use decomposition solution. The introduction of the multiple-use decomposition solution includes a first introduction and a subsequent second introduction. The amount of the decomposed substance in the decomposition solution introduced at the time of first introduction is more than the amount of the decomposed substance in the decomposition solution introduced at the time of second introduction.
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Description

[Technical field]

[0001] The present invention relates to a refinery apparatus and a method for controlling the refinery apparatus. [Background technology]

[0002] In order to recover the target components, a mixed sample containing the components is purified. Non-Patent Document 1 discloses a purification device that recovers microplastics contained in a mixed sample collected from the sea by gravity separation using a heavy liquid. [Prior art documents] [Non-patent literature]

[0003] [Non-Patent Document 1] Hannes K. Imhof et al.,"A novel, highly efficient method for the separation and quantification of plastic particles in sediments of aquatic environments",LIMNOLOGY and OCEANOGRAPHY:METHODS,Volume10,Issue7,pp.524-537,17 July 2012,https: / / doi.org / 10.4319 / lom.2012.10.524 Summary of the Invention [Problem to be solved by the invention]

[0004] In such a refiner, before gravity separation using a heavy liquid, impurities contained in a mixed sample are decomposed using a decomposition liquid. In the decomposition using the decomposition liquid, if a high concentration decomposition liquid is added to a sample with a large amount of impurities remaining, bubbles may be generated due to an overreaction, which may hinder subsequent reactions. On the other hand, if the concentration of the decomposition liquid is too low, the decomposition reaction may not proceed smoothly and may not be completed within the time. In view of this situation, a method for appropriately completing the decomposition using the decomposition liquid and reducing the remaining impurities has been desired. [Means for solving the problem]

[0005] A purification device according to a first aspect of the present disclosure is a purification device for purifying a sample, and includes a container and a control device. The container contains a sample, and a decomposition liquid containing a decomposition substance for decomposing impurities in the sample is introduced into the container. The control device controls the container to introduce the decomposition liquid multiple times. The multiple introductions of the decomposition liquid include a first introduction and a subsequent second introduction. The amount of the decomposition substance in the decomposition liquid introduced during the second introduction is greater than the amount of the decomposition substance in the decomposition liquid introduced during the first introduction.

[0006] A control method according to a second aspect of the present disclosure is a control method executed by a control device in a purification device that purifies a sample. The purification device includes a container and a control device. The container contains a sample, and a decomposition liquid containing a decomposition substance for decomposing impurities in the sample is introduced into the container. The control device controls the container to introduce the decomposition liquid multiple times, including a first introduction and a second introduction. The control method includes a step of performing a first introduction and a step of performing a second introduction. In the step of performing the second introduction, the amount of the decomposition substance in the decomposition liquid introduced in the second introduction is greater than the amount of the decomposition substance in the decomposition liquid introduced during the first introduction. Effect of the Invention

[0007] According to the purification device of the present disclosure, the decomposition liquid is introduced into the container multiple times, including the first introduction and the subsequent second introduction, and the amount of decomposition substance contained in the decomposition liquid increases with the later introduction. As a result, in the first introduction, in which the sample contains a large amount of undecomposed impurities, decomposition can be performed gently with a relatively small amount of decomposition substance. Then, when the amount of undecomposed impurities is reduced, the remaining impurities can be decomposed reliably by adding a larger amount of decomposition substance than in the first introduction. Therefore, the decomposition by the decomposition liquid can be properly completed, and the remaining impurities in the mixed sample can be reduced. [Brief description of the drawings]

[0008] [Figure 1] FIG. 1 is a diagram illustrating a purification device according to an embodiment. [Diagram 2] FIG. 2 is a diagram for explaining a hardware configuration of a refining device. [Diagram 3] 4 is a flowchart of a refining process performed by the refining device. [Figure 4] 13 is a flowchart of a decomposition process in a comparative example. [Diagram 5] 13 is a flowchart of a decomposition process according to an embodiment. [Figure 6] 4 is a flowchart of a decomposition process according to the first embodiment. [Figure 7] 13 is a flowchart of a decomposition process in the second embodiment. [Figure 8] FIG. 13 is a schematic diagram showing a refining device according to a modified example. [Figure 9] 13 is a flowchart of a decomposition process in a modified example. DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS

[0009] The present embodiment will now be described in detail with reference to the drawings. In the drawings, the same or corresponding parts are designated by the same reference characters and, in principle, descriptions thereof will not be repeated.

[0010] [1. Refining equipment configuration] A main configuration of a purification device 1 according to an embodiment will be described with reference to FIG. 1. FIG. 1 is a schematic diagram of the purification device 1 according to an embodiment. As shown in FIG. 1, the purification device 1 includes a purifier 100 for purifying a mixed sample, and a control device 500 for controlling the purifier 100. The purification device 1 according to the embodiment purifies the mixed sample and recovers components to be recovered that are contained in the mixed sample, by controlling the purifier 100 with the control device 500. "Purification" includes extracting pure substances (components) from a mixture.

[0011] The "mixed sample" to be refined by the refining device 1 may be in any form as long as it contains the components to be recovered. For example, the "mixed sample" may be seawater and sand collected from the sea or the coast, or processed products such as food and cosmetics. In the embodiment, the "mixed sample" is exemplified by seawater and sand collected from the sea or the coast. In the following, the "mixed sample" may also be simply referred to as a "sample".

[0012] The "components" to be collected by the refining apparatus 1 may be any components that can be collected by the refining apparatus 1. For example, the "components" include microplastics, which are fine plastic particles having a size of 5 mm or less. In the embodiment, the "components" are exemplified by microplastics contained in seawater and sand collected from the ocean or coast.

[0013] The purifier 100 includes a container 50 for holding a sample, pipes 11-22, pumps 31-33, solenoid valves 41-43, ports 61-64, a stirrer 71, an agitator 72, a discharge pipe 80, a decomposition liquid reservoir 110, a heavy liquid reservoir 120, a rinse liquid reservoir 130, waste liquid reservoirs 140, 150, a detection filter 210, and a supernatant liquid reservoir 215.

[0014] The pipe 11 connects the decomposition liquid reservoir 110 and the solenoid valve 41. The pipe 12 connects the solenoid valve 41 and the pump 31. The pipe 13 connects the pump 31 and a port 61 provided on the outer periphery of the container 50. In this manner, the decomposition liquid reservoir 110 and the port 61 of the container 50 are connected by the pipes 11, 12, and 13 via the solenoid valve 41 and the pump 31.

[0015] Pipe 14 connects the heavy liquid reservoir 120 and the solenoid valve 42. Pipe 15 connects the solenoid valve 42 and the pump 32. Pipe 16 connects the pump 32 and a port 62 provided on the outer periphery of the container 50. In this way, the heavy liquid reservoir 120 and the port 62 of the container 50 are connected by the pipes 14, 15, and 16 via the solenoid valve 42 and the pump 32.

[0016] The pipe 17 connects the rinsing liquid reservoir 130 and the solenoid valve 41. That is, the solenoid valve 41 is connected to the decomposition liquid reservoir 110 by the pipe 11, and is also connected to the rinsing liquid reservoir 130 by the pipe 14. In this manner, the rinsing liquid reservoir 130 and the port 61 of the container 50 are connected by the pipes 17, 12, and 13 via the solenoid valve 41 and the pump 31.

[0017] The pipe 18 connects the rinse liquid reservoir 130 and the solenoid valve 42. That is, the solenoid valve 42 is connected to the heavy liquid reservoir 120 by the pipe 14, and is also connected to the rinse liquid reservoir 130 by the pipe 18. In this manner, the rinse liquid reservoir 130 and the port 62 of the container 50 are connected by the pipes 18, 15, and 16 via the solenoid valve 42 and the pump 32.

[0018] The pipe 19 connects the waste liquid reservoir 140 and the solenoid valve 43. The pipe 20 connects the solenoid valve 43 and the pump 33. The pipe 21 connects the pump 33 and a port 63 provided on the outer periphery of the container 50. In this manner, the waste liquid reservoir 140 and the port 63 of the container 50 are connected by the pipes 19, 20, and 21 via the solenoid valve 43 and the pump 33.

[0019] The pipe 22 connects the pump 33 to a port 64 provided on the outer periphery of the container 50. That is, the pump 33 is connected to the port 63 of the container 50 by the pipe 21, and is also connected to the port 64 of the container 50 by the pipe 22. In this manner, the waste liquid reservoir 140 and the port 64 of the container 50 are connected by the pipes 19, 20, and 22 via the solenoid valve 43 and the pump 33.

[0020] The pipe 23 connects the waste liquid reservoir 150 and the solenoid valve 43. That is, the solenoid valve 43 is connected to the waste liquid reservoir 140 by the pipe 19, and is also connected to the waste liquid reservoir 150 by the pipe 23. In this manner, the waste liquid reservoir 150 and the port 63 of the container 50 are connected by the pipes 23, 20, and 21 via the solenoid valve 43 and the pump 33. Moreover, the waste liquid reservoir 150 and the port 64 of the container 50 are connected by the pipes 23, 20, and 22 via the solenoid valve 43 and the pump 33.

[0021] The decomposition liquid reservoir 110 stores a decomposition liquid for treating impurities. The "impurities" are foreign matter in the mixed sample other than the components to be collected. In the embodiment, the "impurities" are exemplified by organic impurities having organic properties. The "decomposition liquid" may be any liquid that can decompose the impurities. In the embodiment, the "decomposition liquid" decomposes the organic impurities. For example, the "decomposition liquid" may be an oxidizing agent such as hydrogen peroxide (H2O2) or a mixture of hydrogen peroxide (H2O2) and iron oxide (II) (FeO). When the "mixed sample" is seawater and sand, the "organic impurities" may be wood chips and plankton mixed in the seawater or sand.

[0022] The heavy liquid reservoir 120 stores a heavy liquid for separating the sample by the difference in specific gravity. The "heavy liquid" may be any liquid that separates the sample by the difference in specific gravity. In the embodiment, the "heavy liquid" causes inorganic impurities having inorganic properties to settle by the difference in specific gravity. For example, the "heavy liquid" may be sodium chloride (NaCl), sodium iodide (Nal), zinc chloride (ZnCl2), etc. When the "mixed sample" is seawater and sand, the "inorganic impurities" may be sand, glass, stones, etc. The specific gravity of the "heavy liquid" is set to be larger than the specific gravity of the "components" to be collected by the refining device 1 and smaller than the specific gravity of the "inorganic impurities". For example, when the "components" to be collected by the refining device 1 are microplastics and the "inorganic impurities" are sand, glass, stones, etc., the specific gravity of the "heavy liquid" may be set to be larger than the specific gravity of the microplastics and smaller than the specific gravity of the sand, glass, stones, etc. Specifically, the specific gravity of the "heavy liquid" may be set to about 1.5 to about 1.7.

[0023] The rinse liquid reservoir 130 stores a rinse liquid for cleaning the inside of the container 50. The "rinse liquid" may be any liquid that can be used to clean the inside of the container 50. For example, the "rinse liquid" may be water. The "rinse liquid" has a role of diluting the decomposition liquid introduced into the container 50, in addition to cleaning the inside of the container 50.

[0024] The waste liquid reservoirs 140 and 150 store waste liquids such as the heavy liquid discharged from the container 50, the rinse liquid, and seawater contained in the mixed sample.

[0025] The pump 31 introduces the decomposition liquid sucked from the decomposition liquid reservoir 110 or the rinsing liquid sucked from the rinsing liquid reservoir 130 into the container 50 via the port 61 under the control of the control device 500 .

[0026] The pump 32 introduces the heavy liquid sucked from the heavy liquid reservoir 120 or the rinsing liquid sucked from the rinsing liquid reservoir 130 into the container 50 via the port 62 under the control of the control device 500 .

[0027] The pump 33 , under the control of the control device 500 , draws in the waste liquid from the container 50 via the port 63 or the port 64 , and discharges the waste liquid into the waste liquid reservoir 140 or the waste liquid reservoir 150 .

[0028] The solenoid valve 41 is connected to the pipe 11, the pipe 17, and the pipe 1. 2 The solenoid valve 41 is a control valve provided at the junction of the decomposition liquid introduced from the pipe 11 and the rinse liquid introduced from the pipe 17 at a ratio according to the opening degree of the solenoid valve 41.

[0029] When the ratio of the decomposition liquid and the rinse liquid introduced to the solenoid valve 41 is 1:0, the decomposition liquid in the decomposition liquid reservoir 110 is introduced into the container 50. When the ratio of the decomposition liquid and the rinse liquid introduced to the solenoid valve 41 is 0:1, the rinse liquid in the rinse liquid reservoir 130 is introduced into the container 50. In other words, under the control of the control device 500, the solenoid valve 41 can switch the path connected to the port 61 between the path between the decomposition liquid reservoir 110 and the port 61 of the container 50 (the path via the pipes 11, 12, and 13) and the path between the rinse liquid reservoir 130 and the port 61 of the container 50 (the path via the pipes 17, 12, and 13).

[0030] On the other hand, when the ratio of the decomposition liquid and the rinse liquid introduced into the solenoid valve 41 is not 1:0 or 0:1, the decomposition liquid and the rinse liquid are mixed at that ratio in the solenoid valve 41. That is, the decomposition liquid is diluted with the rinse liquid based on that ratio in the solenoid valve 41. Thus, the control device 500 can control the concentration of the decomposition liquid introduced into the container 50 by controlling the opening degree of the solenoid valve 41.

[0031] Based on the control of the control device 500, the solenoid valve 42 switches the path connected to port 62 between the path between the heavy liquid reservoir 120 and port 62 of the container 50 (path via piping 14, 15, 16) and the path between the rinse liquid reservoir 130 and port 62 of the container 50 (path via piping 18, 15, 16).

[0032] Based on the control of the control device 500, the solenoid valve 43 switches the path connected to the ports 63, 64 between the path between the waste liquid reservoir 140 and the ports 63, 64 of the container 50 (the path via pipes 19, 20, 21 or the path via pipes 19, 20, 22) and the path between the waste liquid reservoir 150 and the ports 63, 64 of the container 50 (the path via pipes 23, 20, 21 or the path via pipes 23, 20, 22).

[0033] The port 61 introduces the decomposition liquid in the decomposition liquid reservoir 110 or the rinsing liquid in the rinsing liquid reservoir 130 sucked by the pump 31 into the container 50. The port 62 introduces the heavy liquid in the heavy liquid reservoir 120 or the rinsing liquid in the rinsing liquid reservoir 130 sucked by the pump 32 into the container 50. The ports 63 and 64 discharge the waste liquid in the container 50 sucked by the pump 33 into the waste liquid reservoir 140 or the waste liquid reservoir 150.

[0034] Filters (not shown) are provided inside the ports 61 to 64 to prevent components contained in the sample from being discharged from the container 50. The filters are meshes having mesh sizes large enough to trap the microplastics to be collected. For example, the filters (mesh) are wire meshes made of SUS (Steel Use Stainless) or membrane filters made of PTFE (polytetrafluoroethylene) (Teflon (registered trademark)). When microplastics are to be collected, the mesh size of the filter (mesh) needs to be large enough to block particles of 0.1 to 5.0 mm, and is preferably about 0.1 mm.

[0035] Stirrer 71 is, for example, a thermostatic stirrer, and is disposed below container 50. Stirrer 71 stirs the sample in container 50 by rotating stirring bar 72 provided in container 50 under the control of control device 500. Furthermore, stirrer 71 applies heat to container 50 from below container 50 under the control of control device 500, thereby keeping the temperature of the sample in container 50 constant.

[0036] The discharge pipe 80 is connected to a discharge port 55 provided at the top of the container 50, and discharges the supernatant liquid of the sample that overflows from the container 50 to the outside.

[0037] The detection filter 210 filters the supernatant of the sample discharged from the discharge pipe 80, thereby recovering the components to be recovered that are contained in the supernatant. The supernatant that has passed through the detection filter 210 is recovered by a supernatant reservoir 215. The detection filter 210 is a mesh having mesh sizes large enough to trap the microplastics to be recovered. For example, the detection filter 210 (mesh) may be made of a SUS wire mesh or PTF. Made of E When microplastics are to be collected, the mesh size of the detection filter 210 (mesh) must be large enough to block particles of 0.1 to 5.0 mm, and is preferably about 0.1 mm.

[0038] The control device 500 may be realized by a general-purpose computer, or may be realized by a computer dedicated to controlling the refiner 100. In addition, a part or all of the control device 500 may be constructed as a dedicated hardware circuit. The control device 500 controls the pumps 31 to 33, the solenoid valves 41 to 43, and the stirrer 71 in the refiner 100.

[0039] [2. Hardware configuration] The hardware configuration of the refining device 1 according to the embodiment will be described with reference to Fig. 2. Fig. 2 is a diagram for explaining the hardware configuration of the refining device 1 according to the embodiment. As shown in Fig. 2, the control device 500 includes, as main hardware elements, a calculation device 501, a memory 502, a communication device 503, a display device 504, an input device 505, a data reading device 506, and a storage 510.

[0040] The arithmetic device 501 is a computer that reads out programs (for example, a control program 511 and an OS (Operating System) 513) stored in the storage 510, and deploys and executes the read out programs in the memory 502. For example, the arithmetic device 501 executes a refining process (described later in FIG. 3) for controlling the refiner 100 by executing the control program 511. The arithmetic device 501 is configured, for example, by a CPU (Central Processing Unit), an FPGA (Field Programmable Gate Array), a GPU (Graphics Processing Unit), or an MPU (Multi Processing Unit). The arithmetic device 501 may be configured by a processing circuitry.

[0041] The memory 502 provides a storage area for temporarily storing program code, work memory, etc., when the arithmetic device 501 executes any program. The memory 502 is configured with a volatile memory such as a DRAM (Dynamic Random Access Memory) or an SRAM (Static Random Access Memory), or a non-volatile memory such as a ROM (Read Only Memory) or a flash memory.

[0042] The communication device 503 transmits and receives data to and from other devices via a network (not shown). The communication device 503 supports any communication method, such as Ethernet (registered trademark), wireless LAN (Local Area Network), Bluetooth (registered trademark), etc.

[0043] The display device 504 is configured, for example, by an LCD (Liquid Crystal Display) or the like, and displays a program design screen, an alert screen in the event of an abnormality, and the like.

[0044] The input device 505 is composed of, for example, a keyboard or a mouse, and is used by a user to input design information, etc., when designing a program. The input device 505 may include a start switch for starting the execution of the purification process by the arithmetic device 501.

[0045] The data reader 506 reads out data stored in a recording medium 507. The recording medium 507 may have other configurations as long as it is capable of recording various types of data, such as a CD (Compact Disc), a DVD (Digital Versatile Disc), or a USB (Universal Serial Bus) memory.

[0046] The storage 510 provides a storage area for storing various data necessary for the refining process and the like. The storage 510 is configured, for example, with a non-volatile memory device such as a hard disk drive (HDD) or a solid state drive (SSD). The storage 510 stores a control program 511, control data 512, and an OS 513.

[0047] The control program 511 is a program in which the details of the purification process are described, and is executed by the arithmetic device 501. The control program 511 may be designed by a user using the input device 505, may be read from a recording medium 507 by a data reading device 506, or may be obtained by the communication device 503 from another device such as a server via a network.

[0048] The control data 512 is data used when the arithmetic device 501 executes the control program 511. For example, the control data 512 includes data such as setting values ​​for controlling the pumps 31 to 33, the solenoid valves 41 to 43, and the stirrer 71. The control data 512 may be input by a user using the input device 505, may be read from the recording medium 507 by the data reading device 506, or may be obtained by the communication device 503 from another device such as a server via a network.

[0049] The OS 513 provides basic functions for the arithmetic device 501 to execute various processes.

[0050] [3. Sample purification] Next, the purification process of the sample will be described with reference to Fig. 3. Fig. 3 is a flowchart of the purification process executed by the purification device 1. Each step shown in Fig. 3 is realized by the arithmetic device 501 of the control device 500 executing the OS 513 and the control program 511. In the figure, "S" is used as an abbreviation for "STEP."

[0051] As preparation, the user introduces a sample into the container 50 of the purification device 1. For example, the user puts the sample into the container 50 from an inlet (not shown). After that, the user performs a start operation using the input device 505 of the control device 500, thereby starting control of the purification device 100 by the control device 500.

[0052] 3, when the control of the purifier 100 by the control device 500 starts, the control device 500 controls the pump 33 and the solenoid valve 43 to discharge the waste liquid in the container 50 through the pipes 20-23 and the ports 63, 64 to the waste liquid reservoir 150 (S1). Note that microplastics and the like to be recovered contained in the sample are not discharged to the outside by the filters provided inside the ports 63, 64, and remain in the container 50.

[0053] Next, the control device 500 performs a decomposition process using a decomposition liquid (S2). Details of S2 will be described later with reference to FIGS.

[0054] Next, the control device 500 stops the pump 33 on the discharge side, and controls the pump 31 and the solenoid valve 41 to introduce the rinsing liquid in the rinsing liquid reservoir 130 into the container 50 via the pipes 17, 12, 13 and the port 61, thereby cleaning the inside of the container 50 (S3). At this time, the control device 500 controls the suction amount of the pump 31 to introduce the amount of rinsing liquid preset by the user into the container 50.

[0055] Next, the control device 500 controls the pump 33 and the solenoid valve 43 to discharge the waste liquid in the container 50 after the rinsing liquid has been introduced into the waste liquid reservoir 150 via the pipes 20-23 and the ports 63, 64 (S4). This causes the inside of the container 50 to be cleaned with the rinsing liquid. Note that microplastics and the like contained in the sample and to be collected remain in the container 50 without being discharged to the outside by the filters provided inside the ports 63, 64. Note that thereafter, the control device 500 may dry the sample by leaving it as it is for a predetermined period of time (for example, one day).

[0056] Next, the control device 500 controls the pump 32 and the solenoid valve 42 to introduce the heavy liquid from the heavy liquid reservoir 120 into the container 50 via the pipes 14-16 and the port 62 (S5). At this time, the control device 500 controls the suction amount of the pump 32 to introduce the amount of heavy liquid that is preset by the user into the container 50.

[0057] Thereafter, the control device 500 leaves the sample as it is for a predetermined period of time (for example, 1 to 3 hours) (S6). When the heavy liquid is introduced into the sample in the container 50 in this manner and left as it is, inorganic impurities contained in the sample settle near the bottom of the container 50 due to the difference in specific gravity.

[0058] Next, the control device 500 again controls the pump 32 and the solenoid valve 42 to introduce the heavy liquid from the heavy liquid reservoir 120 into the container 50 again via the pipes 14-16 and the port 62 (S7). At this time, the control device 500 controls the suction amount of the pump 32 to introduce an amount of heavy liquid preset by the user into the container 50. When the heavy liquid is introduced again into the sample in the container 50 in this manner, the liquid level of the gravity-separated sample gradually rises in the container 50, and the supernatant liquid of the sample eventually reaches the discharge port 55 of the container 50. The supernatant liquid of the sample is then discharged to the outside via the discharge port 55 and the discharge pipe 80.

[0059] The supernatant liquid of the sample discharged through the discharge pipe 80 is filtered by the detection filter 210, and only the waste liquid is collected by the supernatant liquid reservoir 215. Microplastics, which are components with a lower specific gravity than the heavy liquid, remain in the detection filter 210.

[0060] After the microplastics are collected by refining the sample, the control device 500 washes the container 50 as post-processing. Specifically, the control device 500 controls the pump 33 and the solenoid valve 43 to discharge the waste liquid in the container 50 after the microplastics are collected to the waste liquid reservoir 140 via the pipes 19 to 22 and the ports 63 and 64 (S8).

[0061] Next, the control device 500 stops the pump 33 on the discharge side, and controls the pump 32 and the solenoid valve 42 to introduce the rinsing liquid in the rinsing liquid reservoir 130 into the container 50 via the pipes 18, 15, 16 and the port 62, thereby cleaning the inside of the container 50 (S9). At this time, the control device 500 controls the suction amount of the pump 32 to introduce the amount of rinsing liquid preset by the user into the container 50.

[0062] Next, the control device 500 controls the pump 33 and the solenoid valve 43 to discharge the waste liquid in the container 50 after the rinsing liquid has been introduced thereinto, via the pipes 19 to 22 and the ports 63 and 64, to the waste liquid reservoir 140 (S10). As a result, the inside of the container 50 is cleaned with the rinsing liquid.

[0063] [4. Decomposition treatment in comparative example] Fig. 4 is a flowchart of a decomposition process in a comparative example. Each step shown in Fig. 4 is performed in place of S2 in the purification process shown in Fig. 3. In other words, in one implementation example of the comparative example, S101 to S103 in Fig. 4 are performed after S1 in Fig. 3, and S3 to S10 in Fig. 3 are performed after S101 to S103 in Fig. 4 are performed.

[0064] Referring to FIG. 4, the control device 500 stops the pump 33 on the discharge side and controls the pump 31 and the solenoid valve 41 to introduce the decomposition liquid in the decomposition liquid reservoir 110 into the container 50 via the pipes 11-13 and the port 61 (S101).

[0065] Next, the control device 500 controls the stirrer 71 to rotate the stirrer 72 provided in the container 50 while applying a constant heat to the container 50, thereby stirring the sample (S102). The temperature of the container 50 and the rotation speed and rotation time of the stirrer 72 are preset by the user. By stirring the sample in this manner, an oxidation process is performed by the oxidizing agent, and organic impurities contained in the sample are decomposed. Note that, while heating is not necessarily required when stirring the sample, maintaining the temperature of the sample at a constant temperature by heating facilitates decomposition by oxidation process.

[0066] Next, the control device 500 controls the pump 33 and the solenoid valve 43 to discharge the waste liquid contained in the sample after the organic impurities have been decomposed from the container 50 to the waste liquid reservoir 150 via the pipes 20-23 and the ports 63, 64 (S103). Note that microplastics and other substances to be recovered contained in the sample remain in the container 50 without being discharged to the outside due to the filters provided inside the ports 63, 64.

[0067] In the decomposition process in the comparative example shown in FIG. 4, for example, if a high concentration decomposition liquid is added to a sample containing a large amount of impurities, bubbles may be generated due to an overreaction, which may hinder the subsequent decomposition reaction. In this case, the impurities in the sample may not be completely decomposed. Conversely, if the concentration of hydrogen peroxide solution is too low, the decomposition may proceed too slowly and may not be completely decomposed within the time. Therefore, in the purification device 1 according to the present embodiment, the decomposition liquid is introduced multiple times, and the amount of decomposition material in the decomposition liquid is controlled so that the amount of decomposition material in the subsequent decomposition liquid is greater. As a result, when the previous introduction, in which the amount of impurities in the sample is large, is less decomposition material than the subsequent introduction, the reaction can be carried out gently. Also, when the subsequent introduction is performed in a state in which the amount of undecomposed impurities is reduced due to the previous introduction, the remaining impurities can be thoroughly decomposed by a larger amount of decomposition material than the previous introduction. As a result, the amount of remaining impurities after the decomposition process can be reduced.

[0068] [5. Decomposition Processing in the Present Embodiment] 5 is a flowchart of the decomposition process in the embodiment. Each step shown in FIG.

[0069] Each step shown in Fig. 5 corresponds to a subroutine of S2 in Fig. 3. In other words, the arithmetic device 501 performs S21 to S26 in Fig. 5 after S1 in Fig. 3, and then performs S3 to S10 in Fig. 3.

[0070] 5, in S21, the arithmetic device 501 controls the pump 31 and the solenoid valve 41 to introduce a first amount of the decomposition substance into the container 50. Hereinafter, this introduction will be referred to as a first introduction.

[0071] In S22, the arithmetic device 501 controls the stirrer 71 to rotate the stirrer 72 provided in the container 50 while applying a constant heat to the container 50, thereby stirring the sample. The temperature of the container 50 and the rotation speed and rotation time of the stirrer 72 are preset by the user. By stirring the sample in this manner, an oxidation process using an oxidizing agent is performed, and organic impurities contained in the sample are decomposed. Note that, while heating is not necessarily required when stirring the sample, maintaining the temperature of the sample at a constant temperature by heating facilitates decomposition by oxidation process.

[0072] In S23, the arithmetic device 501 controls the pump 33 and the solenoid valve 43 to discharge the decomposition liquid from the container 50.

[0073] In S24, the arithmetic device 501 controls the pump 31 and the solenoid valve 41 to introduce a second amount of the decomposition substance, which is greater than the first amount, into the container 50. Hereinafter, this introduction will be referred to as a second introduction.

[0074] In S25, the computing device 501 controls the stirrer 71 to rotate the stirring bar 72 provided in the container 50 while applying a constant heat to the container 50, thereby stirring the sample. The temperature of the container 50 and the rotation speed and rotation time of the stirring bar 72 are, for example, the same as those set values ​​in S22, but may be different.

[0075] In S26, the arithmetic device 501 controls the pump 33 and the solenoid valve 43 to discharge the decomposition liquid from the container 50.

[0076] According to the process shown in Fig. 5, in the first introduction, a first amount of decomposition substance, which is less than the second amount, is introduced so as not to cause an overreaction with the impurities in the sample, and the reaction can proceed gently. Then, in the second introduction, when the impurities have been reduced, a second amount of decomposition substance, which is greater than the first amount, is introduced, so that the remaining impurities can be decomposed reliably. This makes it possible to reduce the amount of impurities remaining after the decomposition process.

[0077] Also, the number of introductions is not limited to two, and may be three or more. For example, one or more introductions of the decomposition liquid may be performed at least one of before the first introduction, between the first introduction and the second introduction, and after the second introduction. In this case, the computing device 501 controls so that the amount of the decomposition substance introduced in the subsequent introduction is greater than that in the previous introduction.

[0078] Furthermore, as shown in FIG. 5, after introducing the decomposition liquid and carrying out the decomposition treatment for a predetermined period of time, it is desirable to discharge the decomposition liquid from the container 50 before introducing the next one. This is to prevent the decomposition liquid introduced during the next introduction from being diluted with the decomposition liquid introduced during the previous introduction. Also, by discharging the impurities decomposed during the previous introduction, it is possible to prevent these impurities decomposed during the previous introduction from interfering with the decomposition reaction during the next introduction. However, if the decomposition liquid introduced during the next introduction contains a relatively large amount of decomposition substances, and the impurities from the previous introduction are diluted, the decomposition liquid may be easily diluted. Decomposition Even if impurities are diluted with liquid or decomposed, Decomposition If the decomposition ability is kept higher than that of the liquid, it is not essential to drain the decomposition liquid before introducing the next liquid.

[0079] The amount of the decomposition substance in the decomposition liquid during these multiple introductions is controlled, for example, by the amount and / or concentration of the decomposition liquid. Next, the control of the amount and concentration of the decomposition liquid will be described.

[0080] (5-1. First embodiment) First, a method of controlling the amount of decomposition substances by controlling the amount of decomposition liquid will be described. FIG. 6 is a flowchart of the decomposition process in the first embodiment. In FIG. 6, S21 and S24 in FIG. 5 are changed to S21A and S24A. S21A and S24A in FIG. 6 are an example of realizing S21 and S24 in FIG. 5. The other steps in FIG. 6 correspond to the other steps in FIG. 5, so the description will be omitted. S21A and S24A are realized by the arithmetic device 501 of the control device 500 executing the OS 513 and the control program 511.

[0081] In S21A, the arithmetic device 501 controls the pump 31 and the solenoid valve 41 to introduce a first amount of decomposition liquid into the container 50. Specifically, the arithmetic device 501 controls the pump 31 to rotate at a predetermined rotation speed and for a predetermined rotation time corresponding to the first amount of liquid. The arithmetic device 501 also controls the opening degree of the solenoid valve 41 to a predetermined opening degree. In one implementation example, the arithmetic device 501 controls the opening degree of the solenoid valve 41 so that only the decomposition liquid in the decomposition liquid reservoir 110 is introduced into the container 50. The decomposition substances in the first amount of decomposition liquid correspond to a first amount.

[0082] In S24A, the arithmetic device 501 controls the pump 31 and the solenoid valve 41 to secondly introduce a second amount of decomposition liquid, which is greater than the first amount, into the container 50. The concentration of the decomposition liquid introduced during the second introduction is controlled to be the same as the concentration of the decomposition liquid introduced during the first introduction. With this configuration, the amount of the decomposition substance introduced during the second introduction is greater than the amount of the decomposition substance introduced during the first introduction.

[0083] Specifically, in S24A, the arithmetic device 501 controls the pump 31 to rotate at a predetermined rotation speed and for a predetermined rotation time corresponding to the second liquid amount. The arithmetic device 501 also controls the opening degree of the solenoid valve 41 to be the same as the predetermined opening degree in S21A. The amount of decomposition substances in the decomposition liquid of the second liquid amount corresponds to the second amount.

[0084] In this manner, the computing device 501 can control the amount of decomposition liquid introduced from the decomposition liquid reservoir 110 to the container 50 by controlling the pump 31, thereby controlling the amount of the decomposition substance.

[0085] In S21A and S24A, the computing device 501 controls the amount of decomposition liquid introduced by controlling the rotation speed and rotation time of the pump 31. With this configuration, the pump 31, which provides the driving force for introducing the decomposition liquid into the container 50, can also be used to control the amount of decomposition liquid introduced. In other words, the amount of decomposition liquid introduced can be controlled with a simple configuration.

[0086] However, the control of the amount of decomposition liquid introduced is not limited to this, and the purifier 100 may be provided with a sensor (not shown) for detecting the amount, and the computing device 501 may control the amount based on the detection value of the sensor. The sensor may be, for example, a liquid amount sensor (e.g., a weight sensor and / or a liquid level sensor) for detecting the amount of liquid in the container 50, a sensor for detecting the amount of decomposition liquid introduced into the container 50 (e.g., a flow rate sensor provided in the pipe 16), and / or a liquid amount sensor for detecting the amount of decomposition liquid remaining in the decomposition liquid reservoir 110. The amount of decomposition liquid may be controlled by preparing two decomposition liquid reservoirs for storing the first and second amounts of decomposition liquid, respectively, and using all of the decomposition liquid in the decomposition liquid reservoir storing the first amount of decomposition liquid in the first introduction, and using all of the decomposition liquid in the decomposition liquid reservoir storing the second amount of decomposition liquid in the second introduction. However, controlling the amount of decomposition liquid introduced into the container 50 from one decomposition liquid reservoir 110 is a simpler configuration for controlling the amount of decomposition liquid introduced into the container 50.

[0087] Furthermore, by controlling the amount of decomposition liquid introduced during the second introduction to be greater than the amount of decomposition liquid introduced during the first introduction, even if part of the sample adheres to the inner wall of the container that was near the liquid level during the decomposition process during the first introduction, the liquid level will be higher during the second introduction, so that the decomposition process can be performed on the adhered sample as well.

[0088] (5-2. Second embodiment) Next, a method of controlling the amount of decomposition substances by controlling the concentration of the decomposition liquid will be described. FIG. 7 is a flowchart of the decomposition process in the second embodiment. In FIG. 7, S21 and S24 in FIG. 5 are changed to S21B and S24B. S21B and S24B in FIG. 7 are an example of realizing S21 and S24 in FIG. 5. The other steps in FIG. 7 correspond to the other steps in FIG. 5, and therefore the description thereof will be omitted. S21B and S24B are realized by the arithmetic device 501 of the control device 500 executing the OS 513 and the control program 511.

[0089] In S21B, the arithmetic device 501 controls the pump 31 and the solenoid valve 41 to introduce the decomposition liquid of the first concentration into the container 50 for the first time. Specifically, the arithmetic device 501 controls the pump 31 to rotate at a predetermined rotation speed and for a predetermined rotation time corresponding to a predetermined liquid amount. The arithmetic device 501 also controls the opening of the solenoid valve 41 to a predetermined opening. In one implementation example, the arithmetic device 501 controls the opening of the solenoid valve 41 so that the rinse liquid several times the amount of the decomposition liquid is introduced into the solenoid valve 41. As a result, the decomposition liquid diluted several times by the rinse liquid is introduced into the container 50. The decomposition substance in the decomposition liquid of the first concentration corresponds to a first amount.

[0090] In S24B, the arithmetic device 501 controls the pump 31 and the solenoid valve 41 to secondly introduce the decomposition liquid having a second concentration higher than the first concentration into the container 50. The amount of the decomposition liquid introduced during the second introduction is controlled to be the same as the amount of the decomposition liquid introduced during the first introduction. With this configuration, the amount of the decomposition substance introduced during the second introduction is greater than the amount of the decomposition substance introduced during the first introduction.

[0091] Specifically, in S24B, the arithmetic device 501 controls the pump 31 to rotate at the same rotation speed and rotation time as in the first introduction. The arithmetic device 501 also controls the opening degree of the solenoid valve 41 so that the ratio of the decomposition liquid is higher than the predetermined opening degree in S21B. In one implementation example, the arithmetic device 501 controls the opening degree of the solenoid valve 41 so that only the decomposition liquid in the decomposition liquid reservoir 110 is introduced into the solenoid valve 41. As a result, the original solution of the decomposition liquid is introduced into the container 50. The amount of the decomposition substance in the second liquid amount of the decomposition liquid corresponds to the second amount.

[0092] In this manner, the arithmetic device 501 can control the concentration of the decomposition liquid introduced into the container 50 by controlling the solenoid valve 41, thereby controlling the amount of the decomposition substance.

[0093] In S21B and S24B, the arithmetic device 501 controls the opening of the solenoid valve 41 to dilute the decomposition liquid with the rinsing liquid at a dilution rate according to the opening, thereby controlling the concentration of the decomposition liquid. With this configuration, the rinsing liquid for cleaning the container 50 can also be used to control the concentration of the decomposition liquid. Moreover, the solenoid valve 41 for switching between introducing the decomposition liquid or the rinsing liquid into the container 50 can also be used to control the concentration of the decomposition liquid introduced into the container 50. That is, the concentration of the decomposition liquid can be controlled with a simple configuration.

[0094] However, the control of the concentration of the decomposition liquid is not limited to this. For example, two decomposition liquid reservoirs may be prepared to store decomposition liquid of a first concentration and a second concentration, respectively, and the decomposition liquid from the decomposition liquid reservoir storing the decomposition liquid of the first concentration may be used in the first introduction, and the decomposition liquid from the decomposition liquid reservoir storing the decomposition liquid of the second concentration may be used in the second introduction.

[0095] Also, a pipe connected to the rinse liquid reservoir 130 may be provided in the container 50 separately from the pipe connected to the decomposition liquid reservoir 110, so that the decomposition liquid and the rinse liquid are introduced into the container 50 and mixed therein. However, the configuration in which the decomposition liquid and the rinse liquid are mixed in the solenoid valve 41 is superior in that the concentration of the decomposition liquid is considered to be approximately uniform when it is added to the sample.

[0096] As shown in Figures 6 and 7, the purification device 1 controls the amount or concentration of the decomposition liquid so that the amount of decomposition substances in the decomposition liquid introduced during the second introduction is greater than the amount of decomposition substances in the decomposition liquid introduced during the first introduction. This allows the decomposition process to be carried out gently in the first introduction, where there is a lot of impurities, and the decomposition process to be completed reliably in the second introduction, where there is a small amount of impurities. This makes it possible to reduce the amount of impurities remaining in the sample after decomposition by the decomposition liquid.

[0097] Naturally, the purification device 1 may control the amount of decomposition substances in the decomposition liquid to be greater during the second introduction than during the first introduction by changing both the amount and concentration of the decomposition liquid introduced into the container 50.

[0098] [6. Modifications] In a modified example, prior to the decomposition process using the decomposition liquid described in the above embodiment, a process is performed to determine the amount of decomposition substance to be introduced in each of the first and second introductions based on at least one of the amount of sample contained in container 50 and the amount of impurities in the sample.

[0099] 8 is a diagram showing a schematic diagram of a refinery apparatus according to a modified example. A refiner 100A of the refinery apparatus 1A in FIG. 8 includes a weight sensor 95 in addition to the configuration of the refiner 100 of the refinery apparatus 1 in FIG.

[0100] Weight sensor 95 is a sensor that detects the weight of the substance contained in the container. A detection value of weight sensor 95 is transmitted to control device 500. A process performed by control device 500 upon receiving the detection value will be described with reference to FIG.

[0101] Fig. 9 is a flowchart of the decomposition process in the modified example. In the flowchart of Fig. 9, S17 to S20 are added before S21 in the flowchart of Fig. 5. S17 to S20 are realized by the arithmetic device 501 of the control device 500 executing the OS 513 and the control program 511.

[0102] In S17, the arithmetic device 501 receives and stores the detection value of the weight sensor 95. In S18, the arithmetic device 501 calculates the amount of the sample and / or the amount of impurities based on the detection value. In one implementation example, the ratio of impurities in the sample is stored in the recording medium 507 in the control device 500. The arithmetic device 501 first calculates the amount of the sample based on the detection value. Then, the arithmetic device 501 multiplies the ratio of impurities with respect to the calculated amount of the sample by Ride The amount of impurities is calculated by this calculation.

[0103] In S19, the arithmetic device 501 determines the amount of decomposition substance to be introduced in each of the first introduction and the second introduction based on the amount of the sample and / or the amount of the impurities. In one implementation example, in the control device 500, data showing the relationship between the "amount of the sample and / or the impurities" and the "amount of the decomposition substance that is preferably introduced in each of the first introduction and the second introduction" is stored in the recording medium 507. The data showing the relationship is stored in the form of, for example, a formula, a graph, or a table. The arithmetic device 501 reads out the "amount of the decomposition substance that is preferably introduced in each of the first introduction and the second introduction" corresponding to the calculated "amount of the sample and / or the amount of the impurities" in the data showing the relationship. Then, the control device 500 determines the "amount of the decomposition substance that is preferably introduced in each of the first introduction and the second introduction" as the amount of the decomposition substance to be introduced in each of the first introduction and the second introduction.

[0104] In S20, the arithmetic device 501 determines the control of the pump 31 and the solenoid valve 41 for each of the first and second introductions based on the amount of the decomposition substance introduced in each of the first and second introductions. In one implementation example, the arithmetic device 501 determines the amount and concentration of the decomposition liquid introduced in each of the first and second introductions based on the amount of the decomposition substance introduced in each of the first and second introductions. Then, the arithmetic device 501 determines the rotation speed and rotation time of the pump 31 and the opening degree of the solenoid valve 41 that realize the amount and concentration of the decomposition liquid introduced in each of the first and second introductions.

[0105] The sensor for detecting the amount of sample contained in the container may be a sensor for detecting the amount of impurities in the sample. These sensors are not limited to weight sensor 95, and may be, for example, a liquid level sensor (not shown) provided in container 50. Also, other sensors such as a concentration sensor or turbidity sensor (not shown) provided in container 50 may be used in combination.

[0106] Also, a sensor for detecting at least one of the amount of sample contained in container 50 and the amount of impurities in the sample may be included outside of purification apparatus 1A, and purification apparatus 1A may acquire a detection value of the sensor and perform the processes from S18 onward. As a more specific example, a user may use a sensor outside purification apparatus 1A to measure at least one of the amount of sample and the amount of impurities in the sample and input the measurement value to purification apparatus 1A. However, a configuration in which purification apparatus 1A is provided with a sensor that automatically detects at least one of the amount of sample contained in container 50 and the amount of impurities in the sample is superior in that it saves the effort of acquiring the detection value.

[0107] In this way, the purification device 1A according to the modified example can detect at least one of the amount of the sample introduced into the container 50 and the amount of impurities in the sample by the sensor. The purification device 1A can then determine the amount of decomposition material to be introduced in each of the first introduction and the second introduction based on at least one of the amount of the sample and the amount of impurities in the sample. This saves the user the trouble of manually calculating the amount of decomposition material to be introduced in each of the first introduction and the second introduction based on the amount of the sample and the amount of impurities in the sample. This makes it easier for the user to use the purification device 1 to properly complete the decomposition by the decomposition liquid and reduce the remaining impurities in the mixed sample.

[0108] As explained in FIG. 3, in the purification apparatus 1, 1A, after the decomposition liquid is discharged in the final step of the decomposition process in the container 50 (S26 in FIGS. 5 to 7), the container 50 is automatically washed, and then a heavy liquid is automatically introduced into the container 50 to perform gravity separation of the sample. In the purification apparatus 1, 1A, the residual impurities are reduced by the decomposition process in the embodiment and the modified example, so that the possibility that the residual impurities will hinder the processes after the gravity separation process is also reduced. By reliably performing the decomposition process, the subsequent analysis error is reduced, and the effort of analyzing unnecessary impurities is saved. That is, the efficiency of the entire purification process in the purification apparatus 1, 1A is improved.

[0109] [Aspects] It will be appreciated by those skilled in the art that the exemplary embodiments described above are examples of the following aspects.

[0110] (Item 1) A purification device according to one embodiment is a purification device for purifying a sample, and includes a container and a control device. The container holds a sample, and a decomposition liquid containing a decomposition substance for decomposing impurities in the sample is introduced into the container. The control device controls the introduction of the decomposition liquid into the container multiple times. The multiple introductions of the decomposition liquid include a first introduction and a subsequent second introduction. The amount of the decomposition substance in the decomposition liquid introduced during the second introduction is greater than the amount of the decomposition substance in the decomposition liquid introduced during the first introduction.

[0111] According to the purification device described in paragraph 1, the decomposition liquid is introduced into the container multiple times, including the first introduction and the subsequent second introduction, and the amount of decomposition substance contained in the decomposition liquid increases with the later introduction. As a result, in the first introduction, in which the sample contains a large amount of undecomposed impurities, decomposition can be performed gently with a relatively small amount of decomposition substance. Then, when the amount of undecomposed impurities is reduced, the remaining impurities can be decomposed reliably by adding a larger amount of decomposition substance than in the first introduction. Therefore, the decomposition by the decomposition liquid can be properly completed, and the amount of remaining impurities in the mixed sample can be reduced.

[0112] (Item 2) In the purification apparatus described in item 1, the control device controls so that after the first introduction, decomposition treatment is performed for a predetermined period of time, the decomposition liquid is discharged from the vessel, and then the second introduction is performed.

[0113] According to the purification device described in the second aspect, it is possible to prevent the decomposition liquid introduced during the second introduction from being diluted with the decomposition liquid introduced during the first introduction. In addition, by discharging the impurities decomposed during the first introduction, it is possible to prevent these decomposition-treated impurities from interfering with the decomposition reaction during the next introduction.

[0114] (Item 3) In the purification apparatus described in items 1 or 2, the control device controls the amount of decomposition liquid introduced during the second introduction to be greater than the amount of decomposition liquid introduced during the first introduction, thereby controlling the amount of decomposition substance introduced during the second introduction to be greater than the amount of decomposition substance introduced during the first introduction.

[0115] According to the purification device described in paragraph 3, by controlling the amount of decomposition liquid, it is possible to make the amount of decomposition substance introduced during the second introduction greater than the amount of decomposition substance introduced during the first introduction.

[0116] (Item 4) The purification device described in item 3 further includes a decomposition liquid reservoir for storing the decomposition liquid introduced into the container. The control device controls the amount of the decomposition liquid introduced from the decomposition liquid reservoir into the container so that the amount of the decomposition liquid introduced into the container from the decomposition liquid reservoir is greater at the time of the second introduction than at the time of the first introduction.

[0117] According to the purification device described in paragraph 4, the purification device controls the amount of decomposition liquid introduced into the container from the decomposition liquid reservoir so that the amount of decomposition liquid introduced into the container at the second introduction is greater than that at the first introduction, thereby making it possible to control the amount of decomposition liquid introduced into the container with a simple configuration.

[0118] (Item 5) The purification apparatus described in item 4 further includes a pump for introducing the decomposition liquid from the decomposition liquid reservoir into the container. The control device controls the amount of decomposition liquid introduced into the container by controlling the number of revolutions and the rotation time of the pump.

[0119] According to the purification device described in the fifth aspect, the pump for providing the driving force for introducing the decomposition liquid into the container can also be used to control the amount of the decomposition liquid to be introduced. In other words, the amount of the decomposition liquid to be introduced can be controlled with a simple configuration.

[0120] (Item 6) In the purification apparatus described in any one of Items 1 to 5, the control device controls the concentration of the decomposition liquid introduced during the second introduction to be higher than the concentration of the decomposition liquid introduced during the first introduction, thereby controlling the amount of the decomposition substance introduced during the second introduction to be greater than the amount of the decomposition substance introduced during the first introduction.

[0121] According to the purification device described in paragraph 6, by controlling the concentration of the decomposition liquid, it is possible to make the amount of decomposition substance introduced during the second introduction greater than the amount of decomposition substance introduced during the first introduction.

[0122] (Item 7) The purification apparatus described in item 6 further includes a rinse liquid reservoir for introducing a rinse liquid for rinsing the inside of the container. The control device controls the concentration of the decomposition liquid introduced into the container by mixing the decomposition liquid and the rinse liquid introduced from the rinse liquid reservoir at a predetermined ratio.

[0123] According to the purification device described in the seventh aspect, the rinse liquid for washing the container can also be used to control the concentration of the decomposition liquid. That is, the concentration of the decomposition liquid can be controlled with a simple configuration.

[0124] (Item 8) The refining apparatus according to item 7 further includes a regulator valve capable of controlling the mixing ratio by controlling the opening degree. The control device controls the mixing ratio by controlling the opening degree.

[0125] According to the purification device described in item 8, the concentration of the decomposition liquid introduced into the container can be controlled by controlling the adjustment valve. In addition, the adjustment valve for switching between introducing the decomposition liquid or the rinse liquid into the container can also be used to control the concentration of the decomposition liquid introduced into the container. In other words, the concentration of the decomposition liquid can be controlled with a simple configuration.

[0126] (Item 9) In the purification device described in any one of items 1 to 8, the control device determines the amount of decomposition substance to be introduced in each of the first introduction and the second introduction based on at least one of the amount of sample introduced into the container and the amount of impurities in the sample.

[0127] The purification device described in paragraph 9 saves the user the trouble of manually calculating the amount of decomposition substance to be introduced in each of the first introduction and the second introduction based on the amount of the sample and the amount of impurities in the sample. This makes it easier for the user to use the purification device to properly complete the decomposition with the decomposition liquid and reduce the amount of impurities remaining in the mixed sample.

[0128] (Item 10) The purification device according to item 9 further comprises a sensor for detecting at least one of the amount of sample introduced into the container and the amount of impurities in the sample.

[0129] According to the purification device described in paragraph 10, the user can reduce the effort required for obtaining detection values ​​compared to when the user uses an external sensor to measure at least one of the amount of the sample and the amount of impurities in the sample and inputs the measurement value into the purification device.

[0130] (Item 11) The purification device according to any one of Items 1 to 10 separates and purifies the sample by gravity separation using a heavy liquid after completion of decomposition of impurities by the decomposition liquid.

[0131] According to the purification device described in paragraph 11, the purification device can also be applied to a purification device using gravity separation. In addition, after the decomposition process in the container, there is no need to transfer the sample to another container for gravity separation after discharging the decomposition liquid. In addition, since the amount of remaining impurities is reduced in the decomposition process, the possibility that the remaining impurities will hinder the process after the gravity separation process is also reduced. By performing the decomposition process reliably, the subsequent analysis error is reduced and the effort of analyzing unnecessary impurities is saved. In other words, the efficiency of the entire purification process is improved.

[0132] (Item 12) A control method according to another aspect is a control method executed by a control device in a purification device that purifies a sample. The purification device includes a container and a control device. The container contains a sample, and a decomposition liquid containing a decomposition substance for decomposing impurities in the sample is introduced into the container. The control device controls the container to introduce decomposition liquid multiple times, including a first introduction and a second introduction. The control method includes a step of performing a first introduction and a step of performing a second introduction. In the step of performing the second introduction, the amount of decomposition substance in the decomposition liquid introduced in the second introduction is greater than the amount of decomposition substance in the decomposition liquid introduced during the first introduction.

[0133] According to the control method described in paragraph 12, the decomposition liquid is introduced into the container multiple times, including the first introduction and the subsequent second introduction, and the amount of decomposition substance contained in the decomposition liquid increases with the later introduction. As a result, in the first introduction, in which the sample contains a large amount of undecomposed impurities, decomposition can be performed gently with a relatively small amount of decomposition substance. Then, when the amount of undecomposed impurities is reduced, the remaining impurities can be decomposed reliably by adding a larger amount of decomposition substance than in the first introduction. Therefore, the decomposition by the decomposition liquid can be properly completed, and the remaining impurities in the mixed sample can be reduced.

[0134] The embodiments disclosed herein should be considered to be illustrative and not restrictive in all respects. The scope of the present invention is defined by the claims, not the above description, and is intended to include all modifications within the scope and meaning equivalent to the claims. [Explanation of symbols]

[0135] 1,1A Purification device, 11,12,13,14,15,16,17,18,19,20,21,22,23 Piping, 31,32,33 Pump, 41,42,43 Solenoid valve, 50 Container, 55 Discharge port, 61,62,63,64 Port, 71 Stirrer, 72 Stirring bar, 80 Discharge pipe, 95 Weight sensor, 100,100A Purification device, 110 Decomposition liquid reservoir, 120 Heavy liquid reservoir, 130 Rinse liquid reservoir, 140,150 Waste liquid reservoir, 210 Detection filter, 215 Supernatant liquid reservoir, 500 Control device, 501 Calculation device, 502 Memory, 503 Communication device, 504 Display device, 505 Input device, 506 Data reading device, 507 Recording medium, 510 storage, 511 control program, 512 control data.

Claims

1. A purification device for purifying a sample, comprising: a container in which a sample is accommodated and into which a decomposition liquid containing a decomposition substance for decomposing impurities in the sample is introduced; a control device for controlling the introduction of the decomposition liquid; The control device controls the container to introduce the decomposition liquid multiple times, The multiple introductions of decomposition liquid include a first introduction and a subsequent second introduction, A purification apparatus, wherein an amount of the decomposed substance in the decomposed liquid introduced during the second introduction is greater than an amount of the decomposed substance in the decomposed liquid introduced during the first introduction.

2. 2. The refining apparatus according to claim 1, wherein the control device controls the second introduction so as to perform decomposition treatment for a predetermined period of time after the first introduction, and then discharge the decomposition liquid from the container.

3. The purification apparatus according to claim 1, wherein the control device controls the amount of decomposition liquid introduced during the second introduction to be greater than the amount of decomposition liquid introduced during the first introduction, thereby controlling the amount of decomposition substance introduced during the second introduction to be greater than the amount of decomposition substance introduced during the first introduction.

4. a decomposition liquid reservoir for storing the decomposition liquid introduced into the container; The purification apparatus according to claim 3 , wherein the control device controls an amount of the decomposition liquid introduced from the decomposition liquid reservoir into the container so that the amount of the decomposition liquid introduced at the second introduction time is greater than the amount of the decomposition liquid introduced at the first introduction time.

5. a pump for introducing decomposition liquid from the decomposition liquid reservoir into the container; The purification apparatus according to claim 4 , wherein the control device controls the amount of the decomposition liquid introduced into the container by controlling a rotation speed and a rotation time of the pump.

6. The purification apparatus according to claim 1, wherein the control device controls the concentration of the decomposition liquid introduced during the second introduction to be higher than the concentration of the decomposition liquid introduced during the first introduction, thereby controlling the amount of the decomposition substance introduced during the second introduction to be greater than the amount of the decomposition substance introduced during the first introduction.

7. a rinse liquid reservoir for introducing a rinse liquid for rinsing the interior of the container; The purification apparatus according to claim 6 , wherein the control device controls a concentration of the decomposition liquid introduced into the container by mixing the decomposition liquid with the rinsing liquid introduced from the rinsing liquid reservoir in a predetermined ratio.

8. Further comprising an adjustment valve capable of controlling the mixing ratio by controlling the opening degree, The refining apparatus according to claim 7 , wherein the control device controls the mixing ratio by controlling the opening degree.

9. 2. The purification device of claim 1, wherein the control device determines an amount of degradant to be introduced in each of the first introduction and the second introduction based on at least one of an amount of sample introduced into the vessel and an amount of contaminants in the sample.

10. 10. The purification device of claim 9, further comprising a sensor for detecting at least one of an amount of sample introduced into the vessel and an amount of a contaminant in the sample.

11. 2. The purification apparatus according to claim 1, wherein after completion of decomposition of the impurities by the decomposition liquid, a heavy liquid is introduced into the container, and the sample is separated and purified by gravity separation using the heavy liquid.

12. a container in which a sample is accommodated and into which a decomposition liquid containing a decomposition substance for decomposing impurities in the sample is introduced; A control method for a purification apparatus for purifying a sample, the method comprising: The control device controls the container to introduce the decomposition liquid a plurality of times, including a first introduction and a second introduction; The control method includes: performing the first introduction; and performing the second introduction, A control method, wherein in the step of performing the second introduction, the amount of the decomposition substance in the decomposition liquid introduced second time is greater than the amount of the decomposition substance in the decomposition liquid introduced during the first introduction.

Citation Information

Patent Citations

  • Separation and purification device for microplastics in marine sediments and using method

    CN109540641A

  • Method for producing optically active sulfoxide compound using aluminum salalen complex catalyst

    JP2008222611A

  • Method for removing iron and aluminum from lithium ion battery scrap

    JP2016191093A