Sample purification apparatus, analysis system, sample purification method, control program

Abstract

The present invention relates to a sample purification apparatus (1), comprising: a container (50) for separating a mixed sample by using a heavy liquid and utilizing the difference in specific gravity; a heavy liquid inlet (12) for introducing the heavy liquid into the container; a discharge section (25) disposed above the heavy liquid inlet in the container in the vertical direction for overflowing the supernatant generated in the container due to the introduction of the heavy liquid to the outside of the container; and a recovery section (21) disposed below the discharge section in the vertical direction for recovering the component of the mixed sample with a specific gravity less than that of the heavy liquid from the supernatant overflowing from the discharge section.

Description

Technical Field

[0001] This disclosure relates to a sample purification apparatus, an analytical system, and a sample purification method. Background Technology

[0002] In the past, in order to recover the component that is to be recovered, the mixed sample containing the component is purified. For example, Non-Patent Document 1 and Non-Patent Document 2 disclose methods for recovering microplastics contained in a mixed sample collected from the sea by purifying the mixed sample.

[0003] Existing technical documents

[0004] Non-patent literature

[0005] Non-patent document 1: "GUIDELINES FOR THE MONITORING AND ASSESSMENT OF PLASTICLITTER IN THE OCEAN", GESAMP Reports and Studies No. 99, National Oceanic and Atmospheric Administration (NOAA), [retrieved June 17, 2020], URL link <URL:https: / / environmentlive.unep.org / media / docs / marine_plastics / une_science_dvision_gesamp_reports.pdf>

[0006] Non-Patent Document 2: "Guidelines for Harmonizing Ocean Surface Microplastic Monitoring Methods", Version 1.0, [Online], May 2019, Ministry of the Environment, [Searched June 17, 2020], URL Link<URL:http: / / www.env.go.jp / en / water / marine_litter / guidelines / guidelines.pdf> Summary of the Invention

[0007] The technical problem that the invention aims to solve

[0008] In the case of recovering microplastics using the sample purification methods disclosed in Non-Patent Literature 1 and Non-Patent Literature 2, manual operations are required in each step of purifying the mixed sample. Furthermore, the mixed sample needs to be transferred between multiple containers. Depending on the specific steps, this process can sometimes take several days, making management extremely difficult and time-consuming for operators. It also carries the risk of deviations in the accuracy of component recovery depending on the skill level of each operator.

[0009] This disclosure was made to address the aforementioned problems and aims to provide a technique for purifying mixed samples with high precision.

[0010] Solution to the above technical problems

[0011] A sample purification apparatus for purifying a mixed sample according to one aspect of the present disclosure comprises: a container for separating the mixed sample using a heavy liquid by means of a specific gravity difference; a heavy liquid inlet for introducing the heavy liquid into the container; a discharge outlet disposed above the heavy liquid inlet in the container in the vertical direction for overflowing the supernatant generated in the container due to the introduction of the heavy liquid to the outside of the container; and a recovery outlet disposed below the discharge outlet in the vertical direction for recovering the components of the mixed sample with a specific gravity less than that of the heavy liquid from the supernatant overflowing from the discharge outlet.

[0012] An analytical system according to one embodiment of the present disclosure includes the aforementioned sample purification apparatus and an analytical apparatus for analyzing the components recovered by the recovery section of the sample purification apparatus.

[0013] According to another aspect of this disclosure, a sample purification method for purifying a mixed sample using a sample purification apparatus equipped with a container, as a computer-executed process, includes: introducing a heavy liquid for separating the mixed sample by means of a specific gravity difference into the container; overflowing the supernatant generated due to the introduction of the heavy liquid to the outside of the container; and recovering the component of the mixed sample with a specific gravity less than that of the heavy liquid from the overflowed supernatant.

[0014] Invention Effects

[0015] According to this disclosure, since mixed samples can be purified by using a continuous operation of a single container, mixed samples can be purified with high precision with minimal operator effort. Attached Figure Description

[0016] Figure 1 This is a schematic diagram illustrating the sample purification apparatus of this embodiment.

[0017] Figure 2 This is a schematic diagram showing the internal structure of the sample purification apparatus of this embodiment.

[0018] Figure 3 This is a diagram illustrating a sample purification method using the sample purification apparatus of this embodiment.

[0019] Figure 4 This is a diagram illustrating a sample purification method using the sample purification apparatus of this embodiment.

[0020] Figure 5 This is a diagram illustrating a sample purification method using the sample purification apparatus of this embodiment.

[0021] Figure 6 This is a diagram illustrating a sample purification method using the sample purification apparatus of this embodiment.

[0022] Figure 7 This is a diagram illustrating a sample purification method using the sample purification apparatus of this embodiment.

[0023] Figure 8 This is a diagram illustrating a sample purification method using the sample purification apparatus of this embodiment.

[0024] Figure 9 This is a diagram illustrating a sample purification method using the sample purification apparatus of this embodiment.

[0025] Figure 10 This is a diagram illustrating a sample purification method using the sample purification apparatus of this embodiment.

[0026] Figure 11 This is a diagram illustrating a sample purification method using the sample purification apparatus of this embodiment.

[0027] Figure 12 This is a diagram illustrating a sample purification method using the sample purification apparatus of this embodiment.

[0028] Figure 13 This is a diagram illustrating a sample purification method using the sample purification apparatus of this embodiment.

[0029] Figure 14 This is a diagram illustrating a sample purification method using the sample purification apparatus of this embodiment.

[0030] Figure 15 This is a diagram illustrating a sample purification method using the sample purification apparatus of this embodiment.

[0031] Figure 16 This is a diagram illustrating a sample purification method using the sample purification apparatus of this embodiment.

[0032] Figure 17This is a flowchart illustrating the sample purification process performed by the sample purification apparatus of this embodiment.

[0033] Figure 18 This is a diagram illustrating the shape of the container of the sample purification apparatus of this embodiment.

[0034] Figure 19 This is a diagram illustrating the shape of the container of the sample purification apparatus of this embodiment.

[0035] Figure 20 This is a diagram schematically illustrating the analysis system of this embodiment.

[0036] Figure 21 This is a schematic diagram illustrating the sample purification apparatus of the second embodiment.

[0037] Figure 22 This is a schematic diagram illustrating the sample purification apparatus of the third embodiment. Detailed Implementation

[0038] This embodiment will be described in detail with reference to the accompanying drawings. Furthermore, the same or corresponding parts in the drawings will be given the same reference numerals, and will generally not be described again.

[0039] [Composition of the Sample Purification Apparatus]

[0040] Figure 1 This diagram schematically illustrates the sample purification apparatus 1 of this embodiment. The sample purification apparatus 1 of this embodiment purifies a mixed sample under the control of a computer 500, thereby performing a process to recover components contained in the mixed sample that are intended for recovery. "Purification" includes making the mixture a pure substance; in this embodiment, it includes obtaining the pure substance (component) intended for recovery from the collected mixed sample.

[0041] The "mixed sample" purified by the sample purification device 1 can be any sample as long as it contains the component to be recovered. For example, examples of "mixed samples" include seawater and sand collected from the sea or coast, processed products such as food and cosmetics. In this embodiment, seawater and sand collected from the sea or coast are used as examples of "mixed samples". In addition, "mixed sample" will be simply referred to as "sample" below.

[0042] The "component" that is recovered by the sample purification device 1 can be any component, as long as it is recovered by the sample purification device 1 of this embodiment. For example, microplastics can be used as a "component". Microplastics are, for example, fine plastic particles with a length of 5 mm or less. In this embodiment, microplastics contained in seawater and sand collected from the sea or coast are used as examples of "components".

[0043] like Figure 1 As shown, the sample purification apparatus 1 includes a sample purifier 100 for purifying samples and a computer 500 for controlling the sample purifier 100.

[0044] The sample purifier 100 includes a container 50, multiple pipes 11 to 15, multiple pumps 31 to 34, multiple ports 61 to 64, a solenoid valve 41, a thermostatic stirrer 71, a stirring element 72, a Peltier element 75, a temperature sensor 80, a camera 90, a discharge pipe 25, a detection filter 21, and a container 210.

[0045] Container 50 is capable of containing a sample. Container 50 is formed of a transparent component such as glass, allowing camera 90 to observe its interior from the outside of container 50. The transmittance of container 50 is set to at least the transmittance required for camera 90 to capture images of the sample contained in container 50.

[0046] Pipe 11 is connected to container 110, through which an oxidant for treating inclusions is introduced from container 110 into port 61 provided in container 50. "Inclusions" are foreign substances other than the components to be recovered in the mixed sample. In this embodiment, organic inclusions having the properties of organic matter are exemplified as "inclusions".

[0047] The "oxidizing agent" can be any substance used to treat impurities. In this embodiment, the "oxidizing agent" decomposes organic impurities. Examples of "oxidizing agents" include hydrogen peroxide water (H2O2), mixtures of hydrogen peroxide water (H2O2) and iron(II) oxide (FeO). When the "mixed sample" is seawater and sand, examples of "organic impurities" include sawdust and plankton mixed in seawater or sand.

[0048] Pipe 12 is connected to container 120, through which heavy liquid for separating samples by gravity difference is introduced from container 120 into port 62 of container 50.

[0049] The "heavy liquid" can be any heavy liquid, as long as it is a substance that separates the sample using a difference in specific gravity. In this embodiment, the "heavy liquid" causes inorganic inclusions with inorganic properties to precipitate due to the difference in specific gravity. Examples of "heavy liquids" include sodium chloride (NaCl), sodium iodide (NaI), and zinc chloride (ZnCl2). When the "mixed sample" is seawater and sand, examples of "inorganic inclusions" include sand, glass, and pebbles. The specific gravity of the "heavy liquid" can be set to be greater than the specific gravity of the "component" that is the target of recovery in the sample purification device 1, and less than the specific gravity of the "inorganic inclusions". For example, when the "component" that is the target of recovery in the sample purification device 1 is microplastics, and the "inorganic inclusions" are sand, glass, and pebbles, the specific gravity of the "heavy liquid" can be set to be greater than the specific gravity of the microplastics, and less than the specific gravity of the sand, glass, and pebbles. Specifically, the specific gravity of the "heavy liquid" can be set to approximately 1.5 to approximately 1.7.

[0050] Pipe 13 is connected to container 130 to introduce rinsing solution for cleaning container 50 from container 130 into port 63 located in container 50.

[0051] The "rinsing solution" can be any rinsing solution used to clean the contents of container 50; for example, water can be used as a "rinsing solution." Furthermore, in this embodiment, the "rinsing solution" introduced through pipe 13 not only cleans the contents of container 50 but also dilutes the oxidant introduced into container 50.

[0052] Pipe 14 is connected to container 140, and discharges the waste liquid in container 50 into container 140 through port 64 located in container 50. Pipe 15 is connected to container 150, and discharges the waste liquid in container 50 into container 150 through port 64 located in container 50.

[0053] Pump 31 is installed between pipe 11 and container 50. Controlled by computer 500, valve 31a is activated to draw in oxidant contained in container 110 and introduce it into port 61. Pump 32 is installed between pipe 12 and container 50. Controlled by computer 500, valve 32a is activated to draw in heavy liquid contained in container 120 and introduce it into port 62. Pump 33 is installed between pipe 13 and container 50. Controlled by computer 500, valve 33a is activated to draw in rinsing solution contained in container 130 and introduce it into port 63. Pump 34 is installed between pipes 14 and 15 and container 50 respectively. Controlled by computer 500, valve 34a is activated to draw in waste liquid from container 50 and discharge it from port 64 into container 140 or container 150. Valves 31a to 34a are examples of "switching units," which switch the flow of liquid by opening and closing the passages of pumps 31 to 34 respectively.

[0054] The "switching unit" can be any component that switches the flow of liquid in and out of pipes 11 to 15. For example, the "switching unit" can be a component that draws in and discharges liquid through the reciprocating motion of a piston or the like, or it can be a component that draws in and discharges liquid through the rotational motion of gears or the like. "Liquid" includes oxidants, heavy liquids, rinsing solutions, and waste liquids.

[0055] Ports 61 to 64 are formed on the outer periphery of container 50 and serve as inlets and outlets for liquid entry and exit. Filters (e.g., described later) are respectively installed inside ports 61 to 64. Figure 19 The filters 163 and 164 shown prevent the components contained in the sample from being discharged to the outside.

[0056] Solenoid valve 41 is installed between pipe 14 and pipe 15 and pump 34 respectively, and is operated by computer 500 to switch the path for waste liquid to pass through between pipe 14 and pump 34 and between pipe 15 and pump 34.

[0057] The thermostatic stirrer 71 is an example of a "stirring section" and a "heating section". A container 50 is placed in the thermostatic stirrer 71. The thermostatic stirrer 71, under the control of a computer 500, rotates a stirring element 72 disposed within the container 50, stirring the sample contained in the container 50. Furthermore, the thermostatic stirrer 71, under the control of the computer 500, heats the sample contained in the container 50. The "heating section" is not limited to a thermostatic stirrer; it can also be any other mechanism capable of heating the sample within the container 50.

[0058] The Peltier element 75 is an example of a "cooling unit". The Peltier element 75 cools the sample contained in the container 50 based on the control of the computer 500. The "cooling unit" is not limited to the Peltier element, but may also be other mechanisms capable of cooling the sample inside the container 50.

[0059] A temperature sensor 80 is disposed, for example, on the bottom surface inside the container 50, to measure the temperature of the sample contained in the container 50. The measured value T of the temperature sensor 80 is output to a computer 500.

[0060] A camera 90 is positioned, for example, outside the container 50, to photograph the sample contained within the container 50. The image data C obtained by the camera 90 is output to the computer 500. The camera 90 is not limited to photographing still images; it can also photograph moving images.

[0061] The discharge pipe 25 is connected to the discharge port 20 located at the top of the container 50, and discharges the supernatant of the sample overflowing from the container 50 to the outside. The discharge port 20 is an example of a "discharge section". The discharge pipe 25 is an example of a "discharge path". The detection filter 21 recovers the components of the recoverable object contained in the supernatant of the sample discharged from the discharge pipe 25 by filtering it. The supernatant that has passed through the detection filter 21 is recovered by the container 210. In a preferred embodiment, the detection filter 21 is a filter capable of capturing microplastics of the recoverable object. Specific examples of this filter are SUS (stainless steel) mesh filters or PTFE (Teflon) membrane filters. The detection filter 21 is an example of a "recovery section".

[0062] Computer 500 can be implemented by a general-purpose computer or by a dedicated computer used to control sample purifier 100. Computer 500 controls valves 31a to 34a, solenoid valve 41, and thermostatic stirrer 71 in sample purifier 100.

[0063] Specifically, the computer 500 drives the motor by supplying electricity to the motor (not shown) through each of the valves 31a to 34a. The driving force of the motor causes the valves 31a to 34a to open and close, thereby enabling the pumps 31 to 34 to draw in and discharge liquid.

[0064] In addition, the computer 500 opens and closes the valve (not shown) by causing current to flow through the solenoid (not shown) of the solenoid valve 41, thereby switching the path through which the waste liquid passes.

[0065] Computer 500 heats the sample contained in container 50 by controlling at least one of the measured value T obtained from temperature sensor 80 and image data C obtained from camera 90, using a thermostatic stirrer 71. Computer 500 drives the motor (not shown) of thermostatic stirrer 71 by supplying electricity to it. The driving force of the motor causes the stirring element 72 to rotate, thereby stirring the sample contained in container 50. Additionally, computer 500 applies constant heat to container 50 by supplying electricity to the heater (not shown) of thermostatic stirrer 71.

[0066] Computer 500 cools the sample contained in container 50 by controlling at least one of the measured values ​​T obtained from temperature sensor 80 and image data C obtained from camera 90 using Peltier element 75.

[0067] Figure 2 This diagram schematically illustrates the internal structure of the sample purification apparatus 1 according to this embodiment. Figure 2As shown, the computer 500 has an arithmetic unit 501, a memory 502, a network controller 503, a display device 504, an input device 505, a data reading device 506, and a storage device 510 as its main hardware components.

[0068] The arithmetic unit 501 is an example of a "control unit". The arithmetic unit 501 is a computational entity that performs various processes by executing various programs. For example, the arithmetic unit 501 executes the sample purification process (by controlling valves 31a to 34a, solenoid valve 41, and thermostatic stirrer 71 in the sample purifier 100) by executing the control program 511 described later. Figure 17 (To be continued).

[0069] The computing device 501 may be composed of, for example, a CPU (Central Processing Unit), an FPGA (Field Programmable Gate Array), or a GPU (Graphics Processing Unit). Alternatively, the computing device 501 may also be composed of a processing circuit for performing calculations.

[0070] In this embodiment, the arithmetic unit 501 of the computer 500 is exemplified as a "control unit," but the "control unit" could also be a controller such as a PLC (programmable logic controller) that sequentially controls each component according to a user-created program. Furthermore, in this embodiment, the "control unit" exists separately from the sample purifier 100, but the "control unit" could also be integrated with the sample purifier 100. For example, a device equivalent to the arithmetic unit 501 could be built into the sample purifier 100.

[0071] The memory 502 provides a storage area for temporarily storing program code or working memory, etc., when the computing device 501 executes any program. The memory 502 is composed of volatile memory devices such as DRAM (Dynamic Random Access Memory) or SRAM (Static Random Access Memory).

[0072] The network controller 503 receives and transmits data with other devices via a network (not shown). The network controller 503 is compatible with any communication method, such as Ethernet (registered trademark), wireless local area network (WLAN), Bluetooth (registered trademark).

[0073] The display device 504 is composed of, for example, an LCD (Liquid Crystal Display) and displays the program design screen and alarm screens in case of abnormalities.

[0074] The input device 505 may consist of, for example, a keyboard and a mouse, and is used by the user to input design information during the design process. The input device 505 may also consist of a start switch for initiating the sample purification process executed by the computing unit 501.

[0075] The data reading device 506 is a device for reading data stored in the storage medium 507. The storage medium 507 can be any medium capable of storing various types of data, such as a CD (Compact Disc), DVD (Digital Versatile Disc), or USB (Universal Serial Bus) memory.

[0076] Storage device 510 provides a storage area for various data required for sample purification and other processes. Storage device 510 is composed of a non-volatile memory device such as a hard disk or SSD (Solid State Drive). Storage device 510 stores control program 511, control data 512, and OS (Operating System) 513.

[0077] Control program 511 is a program that describes the sample purification process and is executed by computing device 501. Control program 511 can be designed by user input device 505, or read from storage medium 507 by data reading device 506, or obtained from server or other devices via network by network controller 503.

[0078] Control data 512 is the data used by the computing device 501 when executing the control program 511. For example, control data 512 includes data for controlling valves 31a to 34a, solenoid valve 41, thermostatic stirrer 71, Peltier element 75, temperature sensor 80, and camera 90. Control data 512 can be input by a user using input device 505, read from storage medium 507 by data reading device 506, or obtained from a server or other device via a network through network controller 503.

[0079] OS513 provides basic functions for performing various processes via the computing device 501.

[0080] [Sample purification method]

[0081] Reference Figures 3 to 16 The sample purification method using sample purification apparatus 1 is described. Figures 3 to 16 This is a diagram illustrating the sample purification method using the sample purification apparatus 1 of this embodiment.

[0082] As a preliminary preparation, the operator and user prepare containers 110, 120, 130, 140, 150, 210, and a detection filter 21. The user places the oxidant in container 110 and inserts pipe 11 into it. The user places the heavy liquid in container 120 and inserts pipe 12 into it. The user places the rinsing solution in container 130 and inserts pipe 13 into it. The user inserts pipe 14 into container 140 and pipe 15 into container 150. At this stage, containers 140 and 150 are empty. Near the outlet of discharge pipe 25, the user sequentially places the detection filter 21 and container 210 from the side of discharge pipe 25.

[0083] like Figure 3 As shown, the user introduces the sample (mixed sample) into the container 50 of the sample purification device 1. For example, the user opens the container 50 by separating a portion of the container 50, which consists of multiple components, and allows the sample to flow into the container 50. Then, the user initiates the operation using the input device 505 of the computer 500, thereby starting control of the sample purifier 100 via the computer 500.

[0084] If the control is initiated by computer 500, then as follows Figure 4 As shown, the computer 500 discharges waste liquid from container 50 to container 140 via control valve 34a and solenoid valve 41, through port 64 and piping 14. The sample contained in container 50 includes waste liquid such as seawater, which is discharged into container 140. On the other hand, microplastics and other materials contained in the sample, which are intended for recycling, are removed by the filter 164 (see reference 140) included in port 64. Figure 19 It cannot be discharged to the outside and remains inside container 50.

[0085] Next, as Figure 5As shown, the computer 500 controls the pump 33 to introduce water contained in container 130 into container 50 via pipe 13 and port 63. At this time, the computer 500 introduces a user-preset amount of water into container 50 by controlling the suction volume of pump 33. For example, the computer 500 controls the suction volume of pump 33 by adjusting the opening degree of valve 33a. Alternatively, the computer 500 may control the suction volume of pump 33 based on the detection value of a liquid level sensor installed in container 130 or container 50. In this embodiment, the rinsing solution (water) used to clean the container 50 is used as a solvent to dilute the oxidant introduced into container 50. Alternatively, the water used to clean the container 50 and the solvent used to dilute the oxidant introduced into container 50 may be contained in different containers and introduced into container 50 via different paths. In this case, the solvent used to dilute the oxidant and the rinsing solution used to clean the container 50 may also be composed of different types of liquids.

[0086] Next, as Figure 6 As shown, the computer 500 introduces the oxidant contained in container 110 into container 50 via control valve 31a, through piping 11 and port 61. At this time, the computer 500 introduces a user-preset amount of oxidant into container 50 by controlling the suction rate of pump 31. For example, the computer 500 controls the suction rate of pump 31 by adjusting the opening degree of valve 31a. Alternatively, the computer 500 may control the suction rate of pump 31 based on the detection value of a liquid level sensor installed in container 110 or container 50.

[0087] Here, if the sample in container 50 contains a substance that acts as a catalyst for the decomposition reaction of an oxidant (such as hydrogen peroxide), such as manganese dioxide or iodine, and the oxidant is added directly to the sample, the decomposition reaction caused by the oxidant may be accelerated, and the oxidant may boil due to the heat generated during the oxidation reaction. If this occurs, the sample may spray out of container 50, or the sample may denature due to heat, which may affect the evaluation and qualitative assessment of the amount of the recovered component (such as microplastics) that is to be recycled. In view of this, in this embodiment, when using... Figure 6 Before introducing the oxidant into container 50 as shown in the steps, by... Figure 5 The steps shown involve introducing water into container 50 beforehand. This dilutes the oxidant introduced into container 50 by mixing with water within container 50, thereby minimizing the risk of a rapid reaction between the sample contained in container 50 and the oxidant.

[0088] Next, as Figure 7As shown, the computer 500 controls the thermostatic stirrer 71 to apply constant heat to the container 50 while rotating the stirring element 72 disposed inside the container 50. The temperature of the container 50 and the rotation speed of the stirring element 72 are preset by the user. By stirring the sample in this way, the oxidant performs oxidation treatment, decomposing the organic inclusions contained in the sample. In addition, heating is not necessarily required when stirring the sample, but maintaining the sample temperature at a constant temperature by heating easily promotes the decomposition caused by oxidation treatment.

[0089] Then, as Figure 8 As shown, the computer 500 cools the sample contained in the container 50 by controlling the Peltier element 75, and adjusts the temperature of the sample to facilitate the oxidation reaction.

[0090] Specifically, the computer 500 acquires the sample temperature measured by the temperature sensor 80 as a measured value T. Based on the measured value T acquired from the temperature sensor 80, the computer 500 controls the Peltier element 75, thereby adjusting the sample temperature. For example, the computer 500 determines whether the sample temperature within the container 50, determined based on the measured value T, is a first temperature. The first temperature is a temperature at which the oxidation reaction of the sample can be appropriately carried out and can be preset by the user. If the sample temperature is not the first temperature, the computer 500 cools the sample contained in the container 50 by controlling the Peltier element 75, so that the sample temperature becomes the first temperature.

[0091] Furthermore, the computer 500 also acquires an image of the sample captured by the camera 90 as image data C. Based on the image data C acquired from the camera 90, the computer 500 controls the Peltier element 75, thereby adjusting the temperature of the sample. For example, the computer 500 determines whether the state of the sample within the container 50, as determined based on the image data C, is abnormal (e.g., over-boiling). If the sample is in an abnormal state, the computer 500 controls the Peltier element 75 to cool the sample contained in the container 50, thus restoring the sample to a normal state. The computer 500 can also determine whether the sample is in an abnormal state by judging whether the liquid level of the sample exceeds a preset threshold, or it can determine whether the sample is in an abnormal state by using AI (Artificial Intelligence) image recognition.

[0092] Alternatively, the computer 500 can control the Peltier element 75 based on at least one of the measured value T from the temperature sensor 80 and the image data C from the camera 90. That is, the computer 500 can control the Peltier element 75 based solely on the measured value T from the temperature sensor 80, or solely on the image data C from the camera 90, or it can control the Peltier element 75 based on both the measured value T from the temperature sensor 80 and the image data C from the camera 90.

[0093] Next, as Figure 9 As shown, when the computer 500 detects that the oxidation reaction is complete, it stops heating the sample contained in the container 50 by controlling the thermostatic stirrer 71 and stops the rotation of the stirring element 72.

[0094] Specifically, the computer 500 acquires the sample temperature measured by the temperature sensor 80 as a measured value T. Based on the measured value T acquired from the temperature sensor 80, the computer 500 controls the thermostatic stirrer 71, thereby stopping the heating and stirring of the sample. For example, the computer 500 determines whether the temperature of the sample in the container 50, determined based on the measured value T, exceeds a second temperature. The second temperature is the temperature at which the oxidation reaction of the sample is completed, and can be preset by the user. During the oxidation reaction, due to the heat generated during the oxidation reaction, there is a tendency for the sample temperature to rise relative to the heating temperature of the thermostatic stirrer 71. Therefore, the second temperature can be set as the heating temperature of the thermostatic stirrer 71. If the sample temperature is below the second temperature, the computer 500 determines that the oxidation reaction of the sample is complete, and thereby stops the heating and stirring of the sample by controlling the thermostatic stirrer 71.

[0095] Furthermore, the computer 500 acquires an image of the sample captured by the camera 90 as image data C. Based on the image data C acquired from the camera 90, the computer 500 controls the thermostatic stirrer 71, thereby stopping the heating and stirring of the sample. For example, during an oxidation reaction, there is a tendency for the liquid level of the sample to become unstable due to boiling caused by the heat generated during the oxidation reaction. The computer 500 determines whether the state of the sample in the container 50, as determined based on the image data C, is a stable state (e.g., a state where the oxidation reaction is complete and the liquid level of the sample is stable). If the state of the sample is stable, the computer 500 determines that the oxidation reaction of the sample is complete, and thus stops the heating and stirring of the sample by controlling the thermostatic stirrer 71. The computer 500 can also determine whether the state of the sample is stable by determining whether the height of the liquid level of the sample exceeds a preset determination value, or it can determine whether the state of the sample is stable by using AI (Artificial Intelligence) image recognition.

[0096] Alternatively, the computer 500 can control the thermostatic stirrer 71 based on at least one of the measured value T from the temperature sensor 80 and the image data C from the camera 90. That is, the computer 500 can control the thermostatic stirrer 71 based solely on the measured value T from the temperature sensor 80, solely on the image data C from the camera 90, or based on both the measured value T from the temperature sensor 80 and the image data C from the camera 90.

[0097] Next, as Figure 10 As shown, the computer 500 discharges the waste liquid contained in container 50 after the decomposition of organic inclusions into container 140 via control valve 34a and solenoid valve 41, through port 64 and piping 14. On the other hand, microplastics and other materials contained in the sample that are intended for recycling cannot be discharged to the outside due to the filter 164 contained in port 64, and remain in container 50.

[0098] Next, as Figure 11 As shown, the computer 500 controls the pump 33 to introduce the rinsing solution contained in container 130 into container 50 via piping 13 and port 63. At this time, the computer 500 introduces a user-preset amount of rinsing solution into container 50 by controlling the suction volume of the pump 33. For example, the computer 500 controls the suction volume of the pump 33 by adjusting the opening degree of valve 33a. Alternatively, the computer 500 may control the suction volume of the pump 33 based on the detection value of a liquid level sensor installed in container 130 or container 50.

[0099] Next, as Figure 12 As shown, the computer 500, through control valve 34a and solenoid valve 41, discharges the waste liquid in container 50, after the rinsing solution has been introduced, into container 140 via port 64 and piping 14. This cleans the inside of container 50 with the rinsing solution. On the other hand, microplastics and other materials contained in the sample, which are intended for recycling, cannot be discharged to the outside due to the filter 164 included in port 64, and remain inside container 50.

[0100] Then, computer 500 dries the sample by placing it in its original state for a specified time (e.g., 1 day). Next, as... Figure 13 As shown, the computer 500, via control valve 32a, introduces heavy liquid contained in container 120 into container 50 through piping 12 and port 62. At this time, the computer 500 introduces a user-preset amount of heavy liquid into container 50 by controlling the suction rate of pump 32. For example, the computer 500 controls the suction rate of pump 32 by adjusting the opening degree of valve 32a. Alternatively, the computer 500 may control the suction rate of pump 32 based on the detection value of a liquid level sensor installed in container 120 or container 50.

[0101] By introducing the heavy liquid into the sample in this manner, the inorganic inclusions contained in the sample precipitate to near the bottom of container 50 due to the difference in specific gravity. Meanwhile, the liquid level of the sample after specific gravity separation gradually rises within container 50, and soon the supernatant of the sample reaches the outlet 20 of container 50. Then, the supernatant of the sample is discharged to the outside through outlet 20 and discharge pipe 25. The supernatant of the sample discharged through discharge pipe 25 is filtered by detection filter 21, and only waste liquid is recovered by container 210. Components with a specific gravity lighter than the heavy liquid, i.e., microplastics, remain in detection filter 21. Since this specific gravity separation takes approximately one day, during this period, computer 500 controls the introduction of the heavy liquid into the sample.

[0102] As described above, the sample purification apparatus 1 according to this embodiment can purify samples through continuous operation using a container 50. Specifically, as Figures 3 to 13 As shown, the sample purifier 100, controlled by computer 500, automatically introduces oxidant and heavy liquid into the sample contained in container 50 at appropriate times and within appropriate timeframes, and discharges waste liquid from container 50. Therefore, the user does not need to manually introduce oxidant and heavy liquid into container 50, nor does the user need to discharge waste liquid from container 50. This eliminates the need for user effort and eliminates concerns about deviations in component recovery accuracy based on individual user skill levels, allowing the user to purify samples with high precision and minimal effort.

[0103] After recovering microplastics through sample purification, container 50 is cleaned using post-treatment. Specifically, such as... Figure 14 As shown, the computer 500 discharges the waste liquid in the container 50 after the microplastics have been recycled into the container 150 via the control valve 34a and the solenoid valve 41, through the port 64 and the piping 15.

[0104] Next, as Figure 15 As shown, the computer 500, via control valve 33a, introduces the rinsing solution contained in container 130 into container 50 through piping 13 and port 63. At this time, the computer 500 introduces a user-preset amount of rinsing solution into container 50 by controlling the suction rate of pump 33. For example, the computer 500 controls the suction rate of pump 33 by adjusting the opening degree of valve 33a. Alternatively, the computer 500 may control the suction rate of pump 33 based on the detection value of a liquid level sensor installed in container 130 or container 50.

[0105] Next, as Figure 16 As shown, the computer 500, through control valve 34a and solenoid valve 41, discharges the waste liquid in container 50, which has been introduced with rinsing solution, into container 150 via port 64 and piping 15. Thus, the container 50 is cleaned with rinsing solution.

[0106] As described above, according to the sample purification apparatus 1 of this embodiment, after recovering microplastics, the used container 50 is automatically cleaned by the sample purifier 100 controlled by the computer 500. Therefore, the user does not need to clean the container 50 himself, minimizing effort.

[0107] [Sample purification process]

[0108] Figure 17 This is a flowchart illustrating the sample purification process performed by the sample purification apparatus 1 of this embodiment. Figure 17 The steps shown are implemented by the execution of OS 513 and control program 511 by the arithmetic unit 501 of computer 500. Additionally, in the figure, "S" is used as an abbreviation for "Step (STEP)".

[0109] With a sample introduced into container 50 of sample purification device 1, if a start operation is received using input device 505, computer 500 executes... Figure 17 The sample purification process is shown. For example... Figure 17 As shown, the computer 500 first discharges the waste liquid in the container 50 into the container 140 through the control valve 34a and the solenoid valve 41 (S1).

[0110] Next, the computer 500 determines whether the discharge of waste liquid is complete (S2). For example, the computer 500 determines whether the discharge of waste liquid is complete based on the degree of opening of valve 34a or the detection value of the liquid level sensor installed in container 140 or container 50.

[0111] If the waste liquid discharge is not completed ("No" in S2), the computer 500 repeats the process of S2. On the other hand, if the waste liquid discharge is completed ("Yes" in S2), the computer 500 introduces the water contained in the container 130 into the container 50 through the control valve 33a (S3).

[0112] Next, the computer 500 determines whether the water introduction is complete (S4). For example, the computer 500 determines whether the water introduction is complete based on the degree of opening of the valve 33a or the detection value of the liquid level sensor installed in the container 130 or the container 50.

[0113] If the water introduction is not completed ("No" in S4), the computer 500 repeats the process of S4. On the other hand, if the water introduction is completed ("Yes" in S4), the computer 500 introduces the oxidant contained in the container 110 into the container 50 through the control valve 31a (S5).

[0114] Next, the computer 500 determines whether the introduction of the oxidant is complete (S6). For example, the computer 500 determines whether the introduction of the oxidant is complete based on the degree of opening of the valve 31a or the detection value of the liquid level sensor installed in the container 110 or the container 50.

[0115] If the introduction of the oxidant is not completed ("No" in S6), the computer 500 repeats the process of S6. On the other hand, if the introduction of the oxidant is completed ("Yes" in S6), the computer 500 stirs the sample with the stirring element 72 while applying constant heat to the sample by controlling the constant temperature stirrer 71 (S7).

[0116] Next, the computer 500 controls at least one of the Peltier elements 75 based on the measured value T of the temperature sensor 80 and the image data C of the camera 90, thereby cooling the sample contained in the container 50 and adjusting the temperature of the sample to facilitate the oxidation reaction (S8).

[0117] Then, the computer 500 determines whether the oxidation reaction of the sample is complete (S9). For example, the computer 500 determines whether the oxidation reaction of the sample is complete based on at least one of the measured value T from the temperature sensor 80 and the image data C from the camera 90. Alternatively, the computer 500 may also determine whether the oxidation reaction of the sample is complete based on the measured value from a timer (not shown).

[0118] If the oxidation reaction of the sample is incomplete ("No" in S9), the computer 500 repeats the process in S9. On the other hand, if the oxidation reaction of the sample is complete ("Yes" in S9), the computer 500 stops the heating and stirring of the sample by controlling the thermostatic stirrer 71 (S10). Then, the computer 500 discharges the waste liquid contained in container 50 of the sample after decomposition of organic inclusions into container 140 by controlling valve 34a and solenoid valve 41 (S11).

[0119] Next, the computer 500 determines whether the discharge of waste liquid is complete (S12). For example, the computer 500 determines whether the discharge of waste liquid is complete based on the degree of opening of valve 34a or the detection value of the liquid level sensor installed in container 140 or container 50.

[0120] If the waste liquid discharge is not completed ("No" in S12), the computer 500 repeats the process of S12. On the other hand, if the waste liquid discharge is completed ("Yes" in S12), the computer 500 introduces the rinsing solution contained in the container 130 into the container 50 through the control valve 33a (S13).

[0121] Next, the computer 500 determines whether the introduction of the rinsing solution is complete (S14). For example, the computer 500 determines whether the introduction of the rinsing solution is complete based on the degree of opening of the valve 33a or the detection value of the liquid level sensor installed in the container 130 or the container 50.

[0122] If the introduction of rinsing solution is not completed ("No" in S14), the computer 500 repeats the process of S14. On the other hand, if the introduction of rinsing solution is completed ("Yes" in S14), the computer 500 discharges the waste liquid in the container 50 after the introduction of rinsing solution into the container 140 through the control valve 34a and the solenoid valve 41 (S15).

[0123] Next, the computer 500 determines whether the discharge of waste liquid is complete (S16). For example, the computer 500 determines whether the discharge of waste liquid is complete based on the degree of opening of valve 34a or the detection value of the liquid level sensor installed in container 140 or container 50.

[0124] If the waste liquid discharge is not completed ("No" in S16), the computer 500 repeats the process of S16. On the other hand, if the waste liquid discharge is completed ("Yes" in S16), the computer 500 introduces the heavy liquid contained in the container 120 into the container 50 through the control valve 32a (S17).

[0125] Next, the computer 500 determines whether the introduction of heavy liquid is complete (S18). For example, the computer 500 determines whether the introduction of heavy liquid is complete based on the degree of opening of valve 32a or the detection value of the liquid level sensor installed in container 120 or container 50.

[0126] If the introduction of heavy liquid is not completed (No in S18), the computer 500 repeats the process of S18.

[0127] By introducing heavy liquid in this way, the inorganic inclusions contained in the sample precipitate to near the bottom of container 50 due to the difference in specific gravity. On the other hand, the supernatant of the sample is discharged to the outside through outlet 20 and discharge pipe 25. Then, the supernatant of the sample discharged through discharge pipe 25 is filtered through detection filter 21, thereby recovering microplastics through detection filter 21.

[0128] After the introduction of heavy liquid is completed ("Yes" in S18), that is, after the microplastics are recovered by gravity separation for about 1 day, the computer 500 discharges the waste liquid in the container 50 after the microplastics have been recovered into the container 150 through the control valve 34a and the solenoid valve 41 (S19).

[0129] Next, the computer 500 determines whether the discharge of waste liquid is complete (S20). For example, the computer 500 determines whether the discharge of waste liquid is complete based on the degree of opening of the valve 34a or the detection value of the liquid level sensor installed in the container 150 or the container 50.

[0130] If the waste liquid discharge is not completed ("No" in S20), the computer 500 repeats the process of S20. On the other hand, if the waste liquid discharge is completed ("Yes" in S20), the computer 500 introduces the rinsing solution contained in the container 130 into the container 50 through the control valve 33a (S21).

[0131] Next, the computer 500 determines whether the introduction of the rinsing solution is complete (S22). For example, the computer 500 determines whether the introduction of the rinsing solution is complete based on the degree of opening of the valve 33a or the detection value of the liquid level sensor installed in the container 130 or the container 50.

[0132] If the introduction of rinsing solution is not completed ("No" in S22), the computer 500 repeats the process of S22. On the other hand, if the introduction of rinsing solution is completed ("Yes" in S22), the computer 500 discharges the waste liquid in the container 50 after the introduction of rinsing solution into the container 150 through the control valve 34a and the solenoid valve 41 (S23), thus ending this process.

[0133] The container is cleaned by post-treatment processes such as introducing rinsing solution and discharging waste liquid.

[0134] As described above, the sample purification apparatus 1 according to this embodiment automatically introduces oxidant and heavy liquid into the sample contained in the container 50 at appropriate times and within appropriate time by executing a control program 511 by a computer 500, and discharges waste liquid from the container 50. Therefore, the user does not need to manually introduce oxidant and heavy liquid into the container 50, nor does the user need to discharge waste liquid from the container 50. Thus, without requiring the user's effort, and without worrying about deviations in the accuracy of component recovery depending on the user's skill level, the user can purify the sample with high accuracy and minimal effort.

[0135] Furthermore, according to the sample purification apparatus 1 of this embodiment, the used container 50 is automatically cleaned after the microplastics are recovered by the control program 511 executed by the computer 500. Therefore, the user does not need to clean the container 50 himself, minimizing the effort required.

[0136] [Shape of the container in the sample purification apparatus]

[0137] Figure 18 and Figure 19This is a diagram illustrating the shape of the container 50 of the sample purification apparatus 1 according to this embodiment. As described above, in the sample purification apparatus 1, sample purification can be performed using the container 50 of the sample purifier 100, but the shape of the container 50 is designed for high-precision sample purification.

[0138] Specifically, such as Figure 18 and Figure 19 As shown, container 50 includes main body portions 51 to 54. Main body portion 51 is an example of a "first main body portion". Main body portion 52 is an example of a "second main body portion". Main body portion 53 is an example of a "third main body portion".

[0139] The main body 54 is located at the bottom of the container and includes a bottom surface 155 and side surfaces 154. The side surfaces 154 of the main body 54 are formed around the central axis 160 of the cylindrical container 50, and a portion therein are holes 156 connected to port 63 and holes 157 connected to port 64. A filter 163 is provided inside port 63. A filter 164 is provided inside port 64. Ports 63 (hole 156) and 64 (hole 157) are respectively formed at positions lower than the central portion of the main body 54 and close to the bottom surface 155. Additionally, although not shown in the figure, filters are also provided inside the other ports 61 and 62.

[0140] The main body 51 is disposed above the main body 54 and includes a side 151 formed immediately adjacent to the side 154 of the main body 54. The side 151 is formed to extend around the central axis 160 of the container 50 and extends downward from the top (outlet 20 side) of the container 50 to the bottom (bottom 155 side).

[0141] The main body 52 is disposed above the main body 51 and includes a side surface 152 formed immediately adjacent to the side surface 151 of the main body 51. The side surface 152 is formed to expand around the central axis 160 of the container 50 and expands from the upper portion 521 and the lower portion 522 of the main body 52 toward the portion located between the upper portion 521 and the lower portion 522. In other words, the side surface 152 is formed to expand from the central axis 160 of the container 50 toward the outer periphery of the main body 52. ​​From another viewpoint, the horizontal cross-sectional area (or inner diameter) of the main body 52 is configured to continuously increase from the upper portion 521 and the lower portion 522 of the main body 52 toward the portion located between the upper portion 521 and the lower portion 522.

[0142] The main body 53 is disposed above the main body 52 and includes a side surface 153 formed immediately adjacent to the side surface 152 of the main body 52. ​​The side surface 153 is formed around the central axis 160 of the container 50 and is tapered from the bottom (bottom surface 155 side) of the container 50 upward (outlet 20 side) towards the tip. From another viewpoint, the horizontal cross-sectional area (or inner diameter) of the main body 53 is configured to continuously decrease in the upward direction toward the outlet 20. In this way, the horizontal cross-sectional area (or inner diameter) of the container 50 is configured to continuously decrease in the upward direction from at least a predetermined height of the container 50 (in this example, the height of the upper part 521 of the main body 52) to the outlet 20. In addition, in this embodiment, the side surface 153 of the main body 53 is a straight line, but the side surface 153 can also be curved, as long as the horizontal cross-sectional area (or inner diameter) of the main body 53 is configured to continuously decrease in the upward direction toward the outlet 20.

[0143] The outlet 20 is a hole formed at a position opposite to the bottom surface 155 of the container 50, adjacent to the side surface 153 of the container 50, and connected to the discharge pipe 25. The horizontal cross-sectional area (or inner diameter) of the outlet 20 is smaller than the horizontal cross-sectional area (or inner diameter) of the upper part 521 and the lower part 522 of the main body 52, respectively.

[0144] The main body 53 and the main body 52 are integrally formed. The main body 52 is separable from the main body 51, and the user can open the container 50 by separating the main body 52 from the main body 51 to allow the sample to flow into the container 50.

[0145] As described above, in the sample purification apparatus 1 according to this embodiment, a portion of the side surface 153 of the container 50 is formed in a conical shape extending from the bottom surface 155 towards the outlet 20. In other words, the horizontal cross-sectional area of ​​the container 50 is configured to continuously decrease upwards from at least a predetermined height of the container 50 to the outlet 20. Therefore, the interface between the side surface 153 of the container 50 and the outlet 20 can be made as smooth as possible. As a result, when the supernatant of the sample separated by gravity due to the heavy liquid is discharged to the outside through the outlet 20, microplastics can be prevented from remaining in the container 50 as much as possible. For example, if the interface between the side surface of the container 50 and the outlet 20 is not smooth and is angular, the supernatant of the sample separated by gravity due to the heavy liquid may come into contact with the angular part, causing the microplastics to be recovered to adhere to the container 50. The microplastics may not flow to the outlet 20 but remain in the container 50. In contrast, by making the junction between the side 153 of container 50 and the outlet 20 as smooth as possible, as in the container 50 of this embodiment, it is possible to minimize the adhesion and retention of microplastics within container 50. Therefore, the user can purify the sample with high precision.

[0146] Because a portion of the side 152 of the container 50 is formed to expand from the upper part 521 and the lower part 522 toward the portion located between the upper part 521 and the lower part 522, it is possible to prevent microplastics from adhering to and remaining inside the container 50 as much as possible. Furthermore, by temporarily expanding the side 152 of a portion of the container 50 (main body 52), and thereby continuously reducing the horizontal cross-sectional area of ​​a portion of the container 50 (main body 53) above it toward the discharge port 20, it is possible to allow the supernatant of the sample rising due to the introduction of heavy liquid to expand in the main body 52, and then to be directed toward the discharge port 20 by the tapering tip of the main body 53.

[0147] Because the main body 53, which tapers to a cone shape, and the main body 52, which expands in an expanded manner, are integrally formed, the strength of the container 50 can be improved. Furthermore, since there is no junction between the main body 53 and the main body 52, the supernatant of the sample rising due to the introduction of heavy liquid will not adhere to the junction between the main body 53 and the main body 52, thereby enabling the supernatant to be directed towards the discharge port 20 more efficiently.

[0148] [Analysis System]

[0149] Figure 20 This is a schematic diagram illustrating the analysis system 1000 of this embodiment. The analysis system 1000 includes the sample purification apparatus 1, the fractionation apparatus 600, and the analysis apparatus 700 described in this embodiment.

[0150] The grading device 600 separates the microplastics recovered by the sample purification device 1 according to particle size. Examples of grading devices 600 include field flow separation devices that use centrifugation to separate particles.

[0151] The analysis device 700 analyzes the microplastics after they have been classified by the grading device 600. The analysis results obtained by the analysis device 700 are displayed on a screen (illustration omitted) and are accessible to the user.

[0152] In the analytical system 1000 configured as described above, microplastics are recovered by the sample purification device 1 under the control of the computer 500, then the microplastics are classified by the grading device 600, and finally analyzed by the analytical device 700.

[0153] As described above, the analysis system 1000 according to this embodiment automates a series of operations from introducing the sample into the sample purification device 1 to analyzing the microplastics through the analysis device 700, thereby improving user convenience.

[0154] Alternatively, the analysis system 1000 may not have a grading device 600; instead, the analysis device 700 may directly acquire and analyze the microplastics recovered by the sample purification device 1.

[0155] [Variation Example]

[0156] The sample purification apparatus 1 and analysis system 1000 of this embodiment have been described above, but various modifications and applications are possible within these configurations. Hereinafter, examples of modifications will be described.

[0157] Figure 21 This is a schematic diagram illustrating the sample purification apparatus 1A of the second embodiment. (See diagram below.) Figure 21 As shown, in the sample purifier 100A of the sample purification apparatus 1A, the pipe 12 for introducing heavy liquid and the pipe 13 for introducing rinsing liquid can also introduce liquids into a common port 62.

[0158] Specifically, pump 232 (valve 232a) and solenoid valve 242 are disposed between pipe 12 and pipe 13 respectively and port 62 of container 50. Solenoid valve 242 is operated by computer 500A to switch the path for liquid to pass through between pipe 12 and pump 232 and between pipe 13 and pump 232.

[0159] Thus, the heavy liquid drawn from container 120 via pipe 12 is introduced into port 62 via solenoid valve 242 and pump 232. In addition, the rinsing solution drawn from container 130 via pipe 13 is introduced into port 62 via solenoid valve 242 and pump 232.

[0160] As described above, in the sample purification apparatus 1A according to the second embodiment, since the pump 232 (valve 232a) provided between the port 62 of the pipe 12 and the container 50 and the pump 232 (valve 232a) provided between the port 62 of the pipe 13 and the container 50 are shared, the number of components of the sample purification apparatus 1A can be reduced to suppress costs.

[0161] Figure 22 This is a schematic diagram illustrating the sample purification apparatus 1B of the third embodiment. (See diagram below.) Figure 22 As shown, the sample purifier 100B of the sample purification apparatus 1B can also be configured to introduce the sample from above the container 50.

[0162] Specifically, the sample purifier 100B includes a discharge pipe 25A that discharges the supernatant of the sample overflowing from container 50 to the detection filter 21, and an inlet pipe 25B that introduces the sample containing microplastics from the outside into container 50. Discharge pipe 25A is an example of a "discharge path," and inlet pipe 25B is an example of an "inlet path." A solenoid valve 45 is disposed between each of the discharge pipe 25A and inlet pipe 25B and the outlet 20 of container 50. The solenoid valve 45 is operated under the control of computer 500B, switching the path for liquid flow between the path between discharge pipe 25A and outlet 20 and the path between inlet pipe 25B and outlet 20.

[0163] Thus, under the control of computer 500B, the supernatant of the sample overflowing from container 50 is discharged to detection filter 21 via solenoid valve 45 and discharge pipe 25A. In addition, under the control of computer 500B, samples introduced from the outside are introduced into container 50 via inlet pipe 25B and solenoid valve 45.

[0164] As described above, the sample purification apparatus 1B according to the third embodiment can provide users with a more convenient sample purification apparatus 1B since it is possible to introduce the sample from above the container 50 using the discharge port 20.

[0165] According to this embodiment, such as Figure 17 As shown, water is introduced into container 50 in advance in S3 before the oxidant is introduced into container 50 in S5. However, in the modified sample purification apparatus, the computer 500 may not perform processes S3 and S4, but instead control valve 31a in process S5, thereby introducing a predetermined amount of oxidant contained in container 110 into container 50 at regular intervals. That is, in order to avoid a sudden mixing of the sample contained in container 50 with the oxidant, the modified sample purification apparatus introduces the oxidant in small, sequential amounts relative to the sample contained in container 50. In this way, the rapid reaction between the sample contained in container 50 and the oxidant can be avoided as much as possible.

[0166] Alternatively, if the computer 500 determines, based on the measured value T obtained from the temperature sensor 80, that the oxidation reaction of the sample has not been fully carried out, it may add the oxidant contained in the container 110 to the container 50 through the control valve 31a.

[0167] Alternatively, if the computer 500 determines, based on the image captured by the camera 90, that the oxidation reaction of the sample has not been fully carried out, it may add the oxidant contained in the container 110 to the container 50 through the control valve 31a.

[0168] [plan]

[0169] Those skilled in the art will understand that the above-described exemplary embodiments are specific examples of the following schemes.

[0170] (Item 1) A sample purification apparatus for purifying a mixed sample according to one embodiment comprises: a container for separating the mixed sample by using a heavy liquid and utilizing the difference in specific gravity; a first pipe for introducing an oxidant for treating inclusions contained in the mixed sample into the container; a second pipe for introducing the heavy liquid into the container; a discharge unit for discharging the supernatant generated in the liquid in the container due to the introduction of the heavy liquid to the outside of the container; a recovery unit for introducing the supernatant discharged from the discharge unit to recover components in the mixed sample whose specific gravity is lighter than that of the heavy liquid; at least one switching unit respectively provided in the first pipe and the second pipe, and switching the inflow and outflow of liquid; and a control unit for controlling the at least one switching unit.

[0171] According to the sample purification apparatus described in item 1, since mixed samples can be purified by continuous operation using a single container, mixed samples can be purified with high precision with minimal effort from the operator or other user.

[0172] (Item 2) In the sample purification apparatus described in Item 1, the sample purification apparatus includes: a third pipe for discharging waste liquid from the container; at least one switching unit disposed on the third pipe for switching the inflow and outflow of liquid; the control unit controls the at least one switching unit disposed on the first pipe, the second pipe, and the third pipe respectively, thereby introducing the oxidant from the first pipe into the container containing the mixed sample, discharging the waste liquid in the container after treating the impurities with the oxidant from the third pipe, and introducing the heavy liquid from the second pipe into the container.

[0173] According to the sample purification apparatus described in item 2, since the mixed sample can be purified by controlling the switching unit through the control unit, the mixed sample can be purified with high precision with minimal effort from the user.

[0174] (Item 3) In the sample purification apparatus described in Item 2, the switching section provided in at least one of the first pipe and the second pipe is different from the switching section provided in the at least one of the third pipe.

[0175] According to the sample purification apparatus described in item 3, since the switching section that allows the liquid to pass through is different for the piping that introduces liquid (oxidant or bleaching liquid) into the container and the piping that discharges waste liquid from the container to the outside, the mixed sample can be purified with higher precision.

[0176] (Item 4) In the sample purification apparatus described in Item 2 or Item 3, the sample purification apparatus includes: a fourth pipe for introducing rinsing solution for cleaning the container into the container; at least one switching unit disposed on the fourth pipe and switching the inflow and outflow of liquid, and the control unit controlling the at least one switching unit disposed on the fourth pipe to introduce the rinsing solution from the fourth pipe into the container from which waste liquid has been discharged.

[0177] According to the sample purification apparatus described in item 4, the container can be cleaned by introducing the rinsing solution into the container from which the waste liquid has been discharged.

[0178] (Item 5) In the sample purification apparatus described in Item 4, the switching unit of the at least one of the second pipes is shared with the switching unit of the at least one of the fourth pipes.

[0179] According to the sample purification apparatus described in item 5, the number of components in the sample purification apparatus can be reduced to suppress costs.

[0180] (Item 6) In the sample purification apparatus described in Item 4 or Item 5, after the control unit discharges the supernatant generated due to the introduction of the heavy liquid to the outside of the container, it controls the at least one switching unit to discharge the waste liquid in the container in which the heavy liquid was introduced from the third pipe, introduce the rinsing solution from the fourth pipe into the container in which the waste liquid was discharged, and discharge the waste liquid in the container in which the rinsing solution was introduced from the third pipe.

[0181] According to the sample purification device described in item 6, after recovering the component to be recovered, the used container is automatically cleaned, so the user does not need to clean the container himself, saving as much effort as possible.

[0182] (Item 7) In any one of the sample purification apparatuses described in items 1 to 6, the sample purification apparatus includes a stirring unit for stirring the mixed sample in the container, and the control unit controls the stirring unit to stir the mixed sample in the container in which the oxidant has been introduced.

[0183] According to the sample purification apparatus described in item 7, since the mixed sample introduced into the container can be uniformly mixed with the oxidant, the mixed sample can be purified with higher precision.

[0184] (Item 8) In the sample purification apparatus described in Item 7, the sample purification apparatus includes a heating unit for heating the mixed sample in the container, and the control unit controls the heating unit to heat the mixed sample in the container in which the oxidant has been introduced.

[0185] According to the sample purification apparatus described in item 8, since the mixed sample introduced into the container can be uniformly mixed with the oxidant while being heated, the mixed sample can be purified with higher precision.

[0186] (Item 9) In any one of the sample purification apparatuses described in items 1 to 8, the sample purification apparatus includes at least one port disposed in the container and through which liquid flows between the container and the at least one switching unit, the at least one port including a filter.

[0187] According to the sample purification apparatus described in item 9, it is possible to prevent the components of the recovered object contained in the mixed sample from being discharged to the outside as much as possible.

[0188] (Item 10) In the sample purification apparatus described in Item 8, the sample purification apparatus includes a temperature sensor for measuring the temperature of the mixed sample inside the container, and the control unit controls the heating unit based on the measurement value of the temperature sensor.

[0189] According to the sample purification apparatus described in item 10, since the sample can be appropriately heated based on its temperature, it is possible to prevent, for example, the sample from being overheated and boiling. Furthermore, since the operator does not need to constantly monitor the progress of the oxidation reaction of the sample, mixed samples can be purified with high precision with minimal effort from the operator or other users.

[0190] (Item 11) In the sample purification apparatus described in Item 8 or Item 10, the sample purification apparatus includes: a cooling unit for cooling the mixed sample in the container; a temperature sensor for measuring the temperature of the mixed sample in the container; and a control unit for controlling the cooling unit based on the measurement value of the temperature sensor.

[0191] According to the sample purification apparatus described in item 11, since the sample temperature can be adjusted to an appropriate temperature based on the sample temperature, it is possible to prevent, for example, the sample from being overheated and boiling. Furthermore, since the operator does not need to constantly monitor the progress of the oxidation reaction of the sample, mixed samples can be purified with high precision with minimal effort from the operator or other users.

[0192] (Item 12) In the sample purification apparatus described in Item 8, the sample purification apparatus includes a camera for photographing the mixed sample in the container, and the control unit controls the heating unit based on the photographed image of the mixed sample acquired by the camera.

[0193] According to the sample purification apparatus described in item 12, since the sample can be appropriately heated based on the state of the sample determined from the photographed image of the sample, it is possible to prevent, for example, the sample from being overheated and boiling. Furthermore, since the operator does not need to constantly observe the progress of the oxidation reaction of the sample, mixed samples can be purified with high precision with minimal effort from the operator or other users.

[0194] (Item 13) In the sample purification apparatus described in Item 8 or Item 12, the sample purification apparatus includes: a cooling unit for cooling the mixed sample in the container; a camera for taking pictures of the mixed sample in the container, and a control unit for controlling the cooling unit based on the pictures of the mixed sample acquired by the camera.

[0195] According to the sample purification apparatus described in item 13, since the temperature of the sample can be adjusted to an appropriate temperature based on the state of the sample determined from the captured image of the sample, it is possible to prevent, for example, the sample from being overheated and boiling. Furthermore, since the operator does not need to constantly observe the progress of the oxidation reaction of the sample, mixed samples can be purified with high precision with minimal effort from the operator or other users.

[0196] (Item 14) In the sample purification apparatus described in Item 2, the sample purification apparatus includes: a fourth pipe for introducing water into the container; at least one switching unit disposed on the fourth pipe and switching the inflow and outflow of liquid, wherein the control unit controls the at least one switching unit disposed on the fourth pipe before introducing the oxidant from the first pipe, thereby introducing the water from the fourth pipe into the container.

[0197] According to the sample purification apparatus described in item 14, by mixing the oxidant introduced into the container with water inside the container, it is possible to minimize the rapid reaction between the sample contained in the container and the oxidant.

[0198] (Item 15) In the sample purification apparatus described in Item 2, the control unit, by controlling the switching unit provided in at least one of the first pipes, introduces the oxidant from the first pipe in a predetermined amount into the container containing the mixed sample at a certain period.

[0199] According to the sample purification apparatus described in item 15, by introducing an oxidant in a predetermined amount relative to the sample contained in the container, it is possible to minimize the rapid reaction between the sample contained in the container and the oxidant.

[0200] (Item 16) An analytical system comprising: the sample purification apparatus described in any one of items 1 to 15; and an analytical apparatus for analyzing the components recovered by the recovery section of the sample purification apparatus.

[0201] According to the analytical system described in item 16, the user's convenience is improved because the series of operations from introducing the mixed sample into the sample purification device to analyzing the components of the recovered object through the analytical device are automated by the control unit.

[0202] (Item 17) A sample purification method for purifying a mixed sample includes the steps of: introducing an oxidant for treating inclusions into a container containing the mixed sample; discharging waste liquid from the container after treating inclusions with the oxidant; introducing a rinsing solution for cleaning the container into the container after the waste liquid has been discharged; introducing a heavy liquid for separating the mixed sample by gravity difference into the container; and discharging the supernatant generated by introducing the heavy liquid to the outside of the container.

[0203] According to the sample purification method described in item 17, since mixed samples can be purified by using a continuous operation of a single container, mixed samples can be purified with high precision with minimal effort from the operator or other users.

[0204] (Item 18) A control program for purifying a mixed sample causes a computer to perform the following steps: introducing an oxidant for treating inclusions into a container containing the mixed sample; discharging waste liquid from the container after treating the inclusions with the oxidant; introducing a rinsing solution for cleaning the container into the container after the waste liquid has been discharged; introducing a heavy liquid for separating the mixed sample by gravity difference into the container; and discharging the supernatant generated by introducing the heavy liquid to the outside of the container.

[0205] According to the control procedure described in item 18, since the mixed sample can be purified by using a continuous operation of a container, the mixed sample can be purified with high precision with minimal effort from the operator or other users.

[0206] Explanation of reference numerals in the attached figures

[0207] 1. Sample purification apparatus (1A, 1B)

[0208] 11, 12, 13, 14, 15 piping

[0209] 20 Discharge section

[0210] 21 Detection Filter

[0211] 25, 25A discharge pipe

[0212] 25B infusion tube

[0213] Pumps 31, 32, 33, 34, and 232

[0214] Valves 31a, 32a, 33a, 34a, 64a, 232a

[0215] 41, 45, 242 Solenoid valves

[0216] Containers of sizes 50, 110, 120, 130, 140, 150, and 210

[0217] 51, 52, 53 Main body

[0218] Ports 61, 62, 63, and 64

[0219] 71 Thermostatic Stirrer

[0220] 72. Mixing component

[0221] 75 Peltier components

[0222] 80 Temperature Sensor

[0223] 90 cameras

[0224] 100, 100A, 100B Sample Purifiers

[0225] 151, 152, 153, 154 Side View

[0226] 155 Bottom

[0227] Holes 156 and 157

[0228] 160 central axis

[0229] Filters 163 and 164

[0230] 500, 500A, 500B Computers

[0231] 501 Computing Device

[0232] 502 Memory

[0233] 503 Network Controller

[0234] 504 Display Device

[0235] 505 Input Device

[0236] 506 Data Reading Device

[0237] 507 Storage Media

[0238] 510 Storage Devices

[0239] 511 Control Procedure

[0240] 512 Control Data

[0241] 521 upper

[0242] 522 lower part

[0243] 600 Grading Device

[0244] 700 Analytical Device

[0245] 1000 Analysis System.

Claims

1. A sample purification apparatus, which is a sample purification apparatus for purifying mixed samples, characterized in that, have: A container for separating the mixed sample using a heavy liquid by utilizing the difference in specific gravity; A heavy liquid inlet is used to introduce the heavy liquid into the container; A discharge section is provided at the top of the container, which is located vertically above the heavy liquid inlet section in the container, for discharging the supernatant generated in the liquid in the container due to the introduction of the heavy liquid to the outside of the container. The discharge path guides the supernatant discharged from the discharge section; A recovery section, disposed below the discharge section in the container in the vertical direction, is used to recover components of the mixed sample that are lighter than the heavy liquid from the supernatant that overflows from the discharge section and is guided by the discharge path. The horizontal cross-sectional area of ​​the container is configured to decrease continuously from at least a predetermined height of the container to the discharge portion as it moves upward.

2. The sample purification apparatus as described in claim 1, characterized in that, have: A decomposing agent introduction section is used to introduce a decomposing agent for treating inclusions contained in the mixed sample into the container; Waste liquid discharge section, used to discharge waste liquid from the container; At least one switching unit is respectively provided in the decomposer inlet, the heavy liquid inlet and the waste liquid outlet, and switches the inlet and outlet of the liquid; The control unit controls the switching unit of at least one of them. The control unit controls the switching unit of at least one of them. This allows the decomposing agent from the decomposing agent inlet to be introduced into the container containing the mixed sample. The waste liquid in the container, after the inclusions have been treated with the decomposing agent, is discharged from the waste liquid discharge section. The heavy liquid is introduced into the container from the heavy liquid inlet.

3. The sample purification apparatus as described in claim 2, characterized in that, The switching section provided in the at least one of the decomposition agent inlet section and the heavy liquid inlet section is different from the switching section provided in the at least one of the waste liquid outlet section.

4. The sample purification apparatus as described in claim 2 or claim 3, characterized in that, have: A rinsing solution inlet is used to introduce rinsing solution for cleaning the container into the container; At least one switching unit is provided at the rinsing liquid inlet, and switches the inflow and outflow of the liquid. The control unit controls the switching unit provided in at least one of the rinsing liquid inlet sections, thereby introducing the rinsing liquid from the rinsing liquid inlet section into the container from which waste liquid has been discharged.

5. The sample purification apparatus as described in claim 4, characterized in that, The switching unit provided in the heavy liquid inlet section is shared with the switching unit provided in the rinsing liquid inlet section.

6. The sample purification apparatus as described in claim 4, characterized in that, After the control unit discharges the supernatant generated due to the introduction of the heavy liquid to the outside of the container, it controls the at least one switching unit. Thus, the waste liquid that had been introduced into the container and then discharged from the waste liquid discharge section is discharged. The rinsing solution is introduced from the rinsing solution inlet into the container from which the waste solution has been discharged. The waste liquid in the container into which the rinsing solution has been introduced is discharged from the waste liquid discharge section.

7. The sample purification apparatus as described in claim 2, characterized in that, The container is equipped with a stirring unit for stirring the mixed sample inside the container. The control unit controls the stirring unit, thereby stirring the mixed sample introduced into the container with the decomposing agent.

8. The sample purification apparatus as described in claim 7, characterized in that, It includes a heating unit for heating the mixed sample inside the container. The control unit controls the heating unit, thereby heating the mixed sample in the container in which the decomposing agent has been introduced.

9. The sample purification apparatus as described in claim 2, characterized in that, The container has at least one port disposed thereon, through which liquid flows in and out between the container and the at least one switching unit. The port of at least one of them contains a filter.

10. The sample purification apparatus as described in claim 8, characterized in that, It is equipped with a temperature sensor to measure the temperature of the mixed sample inside the container. The control unit controls the heating unit based on the measurement value of the temperature sensor.

11. The sample purification apparatus as described in claim 8, characterized in that, have: The cooling section cools the mixed sample inside the container; A temperature sensor measures the temperature of the mixed sample inside the container. The control unit controls the cooling unit based on the temperature sensor's measurements.

12. The sample purification apparatus as described in claim 8, characterized in that, The container is equipped with a camera for photographing the mixed sample inside the container. The control unit controls the heating unit based on images of the mixed sample captured by the camera.

13. The sample purification apparatus as described in claim 8, characterized in that, have: The cooling section cools the mixed sample inside the container; A camera is used to photograph the mixed sample inside the container. The control unit controls the cooling unit based on images of the mixed sample captured by the camera.

14. The sample purification apparatus as described in claim 2, characterized in that, have: A water inlet section is used to introduce water into the container; At least one switching unit is provided at the water inlet section, and switches the inflow and outflow of liquid. Before introducing the decomposer from the decomposer inlet, the control unit controls at least one of the switching units provided in the water inlet, thereby introducing water from the water inlet into the container.

15. The sample purification apparatus as described in claim 2, characterized in that, The control unit controls at least one of the switching units provided in the decomposition agent inlet to introduce the decomposition agent in a predetermined amount from the decomposition agent inlet to the container containing the mixed sample at a certain period.

16. An analysis system, characterized in that, have: The sample purification apparatus as described in claim 1; and An analytical apparatus for analyzing the components recovered by the recovery section of the sample purification device.

17. A sample purification method, which uses a sample purification apparatus equipped with a container to purify a mixed sample, characterized in that, The sample purification method includes, as a computer-executed process: The steps are as follows: a heavy liquid used to separate the mixed sample by means of specific gravity difference is introduced into the container, and the supernatant generated by the introduction of the heavy liquid is discharged from the discharge part provided at the top of the container to the outside via the discharge path. The step of recovering the component of the mixed sample that is lighter than the heavy liquid from the supernatant that overflows from the discharge section and is guided by the discharge path. The horizontal cross-sectional area of ​​the container is configured to continuously decrease from at least a predetermined height of the container to the discharge portion in the upward direction in the vertical direction.

Images