Online sampler

Abstract

The flow path portion has a first end portion and a second end portion disposed in the tank, and circulates the sample stored in the tank. A first end portion and a second end portion of the flow path portion are respectively provided with a filter. The sample introduction part has an introduction port for introducing the sample flowing through the flow path part into the interior, and a discharge port for discharging the sample introduced into the interior to the flow path part. The switching valve is capable of switching between a first connection state in which the sample in the tank is introduced from the first end into the flow path portion and the sample in the flow path portion is introduced from the second end into the tank, and a second connection state in which the sample in the tank is introduced from the second end into the flow path portion and the sample in the flow path portion is introduced from the second end into the tank. The sample in the flow path portion is led out from the first end portion into the tank.

Description

Technical Field

[0001] This invention relates to online samplers. Background Technology

[0002] In the monitoring system, a portion of the product generated through synthesis or reaction is extracted as a sample from a reactor or similar device. The extracted sample is then fed to an analytical apparatus such as an LC (Liquid Chromatography) for analysis. By analyzing the sample, it can be confirmed whether the product has met the specified quality requirements. Patent Document 1 describes an OSM (Online Sample Manager) for real-time extraction of samples from a sample line and supplying them to an LC.

[0003] In the OSM of Patent Document 1, with the processing valve connected to port 1, a sample is drawn from the sample line using a sample injector. Then, with the processing valve connected to port 2, the sample drawn by the sample injector is ejected. This allows the sample to be injected into the sample loop located on the column valve via a cleaning injector or similar device. Afterward, by switching the connection state of the column valve, the sample in the sample loop is supplied to the LC column.

[0004] Patent Document 1: U.S. Patent Application Publication No. 2019 / 0366325 Summary of the Invention

[0005] The technical problem that the invention aims to solve

[0006] Samples generated through synthesis or reaction sometimes have a slurry-like consistency, consisting of a mixture of liquid components and various crystallized solid components. Feeding a sample containing solid components to an LC can cause flow path blockage. Furthermore, if the solid components redissolve within the LC's flow path, the sample concentration will change, making proper sample analysis impossible.

[0007] The purpose of this invention is to provide an online sampler that can properly sample specimens.

[0008] Technical solutions to the problem

[0009] One aspect of the present invention relates to an online sampler comprising: a container for storing a sample; a flow path having a first end and a second end disposed within the container for circulating the sample stored in the container; a first filter installed at the first end of the flow path; a second filter installed at the second end of the flow path; a sample inlet having an inlet port for introducing a sample flowing through the flow path into the interior, and an outlet port for exporting the sample introduced into the interior to an outlet port of the flow path; a first pump for pressurizing the sample flowing through the flow path; and a first switching valve capable of switching between a first connection state and a second connection state, wherein the first connection state is: the sample in the container is introduced from the first end into the flow path, and the sample in the flow path is exported from the second end into the container; and the second connection state is: the sample in the container is introduced from the second end into the flow path, and the sample in the flow path is exported from the first end into the container.

[0010] Invention Effects

[0011] According to the present invention, it is possible to properly sample the specimen. Attached Figure Description

[0012] [ Figure 1 ] Figure 1 This is a diagram showing the structure of the online sampler according to the first embodiment of the present invention.

[0013] [ Figure 2 ] Figure 2 This is a diagram illustrating an example of the cyclical operation of a sample stored in a container.

[0014] [ Figure 3 ] Figure 3 This is a diagram illustrating an example of the cyclical operation of a sample stored in a container.

[0015] [ Figure 4 ] Figure 4 This is a diagram illustrating an example of the sample supply operation to a vial.

[0016] [ Figure 5 ] Figure 5 This is a diagram illustrating an example of the sample supply operation to an analytical apparatus.

[0017] [ Figure 6 ] Figure 6 This is a diagram illustrating an example of the sample supply operation to an analytical apparatus.

[0018] [ Figure 7 ] Figure 7 This is a diagram showing the structure of the online sampler according to the second embodiment of the present invention.

[0019] [ Figure 8 ] Figure 8This is a diagram illustrating an example of the cyclical operation of a sample stored in a container.

[0020] [ Figure 9 ] Figure 9 This is a diagram illustrating an example of the cyclical operation of a sample stored in a container.

[0021] [ Figure 10 ] Figure 10 This is a diagram showing the structure of the online sampler according to the third embodiment of the present invention.

[0022] [ Figure 11 ] Figure 11 This is a diagram illustrating an example of the sample supply operation to a flow vial. Detailed Implementation

[0023] 1. First Implementation Method

[0024] (1) Structure of the online sampler

[0025] Hereinafter, the online sampler according to embodiments of the present invention will be described in detail with reference to the accompanying drawings. Figure 1 This is a diagram illustrating the structure of the online sampler according to the first embodiment of the present invention. Figure 1 As shown, the online sampler 100 includes two filters 101 and 102, a canister 110, a flow path section 120, a sample loop 130, pumps 140 and 150, one or more vials 160, a metering section 170, and an injection port 180, and is connected to the analytical apparatus 200. Additionally, the online sampler 100 includes switching valves 10, 20, 30, and 40 for switching the flow path.

[0026] The online sampler 100 performs real-time sampling of the analyte sample by operating each component of its components. Furthermore, the online sampler 100 may further include a control unit. In this case, the operation of each component of the online sampler 100 is controlled by the control unit. Alternatively, the online sampler 100 may be connected to an external control unit. In this case, the operation of each component of the online sampler 100 is controlled by the external control unit.

[0027] The analytical apparatus 200 is, for example, a liquid chromatograph, including a mobile phase container 210, a pump 220, an analytical column 230, and a detector 240. The mobile phase container 210 stores a mobile phase such as water. The pump 220 introduces the sample of the analyte supplied by the online sampler 100, together with the mobile phase stored in the mobile phase container 210, into the analytical column 230. The analytical column 230 separates the introduced sample into various components based on differences in chemical properties or composition. The detector 240 detects the components of the sample that have passed through the analytical column 230. The detection results obtained from the detector 240 are used to generate a liquid chromatogram.

[0028] The tank 110 of the online sampler 100 stores a sample of the analyte. In this example, the sample is a slurry containing a liquid component of the analyte and various crystallized solid components. The sample is generated, for example, by reacting or synthesizing one or more liquid raw materials.

[0029] The two ends of the flow path 120 are disposed within the tank 110. The sample stored in the tank 110 flows within the flow path 120. Filters 101 and 102 are respectively installed at both ends of the flow path 120 within the tank 110. In this example, the flow path 120 includes multiple (five in this example) pipes 121 to 125. Pipe 121 is located at one end of the flow path 120, and pipe 124 is located at the other end of the flow path 120. Therefore, filter 101 is installed at the end of pipe 121, and filter 102 is installed at the end of pipe 124.

[0030] The sample ring 130 is an example of a sample inlet. The sample ring 130 has an inlet port 131 at one end for introducing the sample into the interior, and an outlet port 132 at the other end for discharging the sample from the interior. The sample ring 130 is inserted into the flow path 120 to temporarily store the introduced sample. The pump 140 pressurizes the sample within the flow path 120 to introduce the sample into the sample ring 130. In this example, the pump 140 is inserted into the piping 122 of the flow path 120. The pump 140 may also be inserted into the piping 123 of the flow path 120. In these cases, the sample flowing through the flow path 120 can be efficiently pressurized by the pump 140.

[0031] Pump 150 pressurizes the sample stored in sample loop 130 toward vial 160. Vial 160 stores the sample discharged from sample loop 130. Pretreatments such as sample dilution, dispensing, or reagent addition can also be performed in vial 160. Metrology unit 170 includes, for example, a sampling needle and a pump. Metrology unit 170 draws the sample stored in vial 160 and injects the drawn sample into injection port 180. The sample injected into injection port 180 is supplied to analytical apparatus 200.

[0032] Switching valves 10, 20, 30, and 40 are, for example, multi-directional switching valves. Switching valve 10 has six ports 11 to 16 and is capable of switching between a first connection state and a second connection state. In the first connection state, ports 11 and 12 are connected, ports 13 and 14 are connected, and ports 15 and 16 are connected. In the second connection state, ports 12 and 13 are connected, ports 14 and 15 are connected, and ports 16 and 11 are connected.

[0033] The switching valve 20 has six ports 21 to 26 and can switch between a third connection state and a fourth connection state. In the third connection state, ports 21 and 22 are connected, ports 23 and 24 are connected, and ports 25 and 26 are connected. In the fourth connection state, ports 22 and 23 are connected, ports 24 and 25 are connected, and ports 26 and 21 are connected.

[0034] The switching valve 30 has six ports 31 to 36 and can switch between a fifth connection state and a sixth connection state. In the fifth connection state, ports 31 and 32 are connected, ports 33 and 34 are connected, and ports 35 and 36 are connected. In the sixth connection state, ports 32 and 33 are connected, ports 34 and 35 are connected, and ports 36 and 31 are connected.

[0035] The switching valve 40 has six ports 41 to 46 and can switch between a seventh connection state and an eighth connection state. In the seventh connection state, ports 41 and 42 are connected, ports 43 and 44 are connected, and ports 45 and 46 are connected. In the eighth connection state, ports 42 and 43 are connected, ports 44 and 45 are connected, and ports 46 and 41 are connected.

[0036] In the switching valve 10, port 11 is connected to one end of pipe 121. Port 12 is connected to one end of pipe 122. Port 13 is connected to one end of pipe 124. Port 14 is connected to one end of pipe 123. Port 15 is connected to one end of pipe 125. Port 16 is connected to the other end of pipe 125. Furthermore, the other ends of pipe 121 and pipe 124 are configured within tank 110 with filters 101 and 102 respectively installed.

[0037] In switching valve 20, port 21 is connected to the other end of piping 122. Port 22 is connected to the inlet port 131 of sample loop 130. Port 23 is connected to pump 150. Port 24 is connected to port 31 of switching valve 30. Port 25 is connected to the outlet port 132 of sample loop 130. Port 26 is connected to the other end of piping 123.

[0038] In switching valve 30, port 31 is connected to port 24 of switching valve 20 as described above. Port 32 is selectively connected to any one of the more than one vial 160. Port 33 is connected to port 44 of switching valve 40. Port 34 is connected to a waste liquid device (not shown). Ports 35 and 36 are not connected.

[0039] In switching valve 40, port 41 is connected to injection port 180. Port 42 is connected to the analysis column 230 of the analysis device 200. Port 43 is connected to the pump 220 of the analysis device 200. Port 44 is connected to port 33 of switching valve 30 as described above. Ports 45 and 46 are not connected. The operation of the online sampler 100 will be described in detail below. The connection states of the switching valves 10, 20, 30, and 40 during various operations of the online sampler 100 are not limited unless specifically mentioned.

[0040] (2) Operation of the online sampler

[0041] Figure 2 and Figure 3 This diagram illustrates an example of the circulation process of a sample stored in container 110. During the sample circulation process, as... Figure 2 As shown, switching valve 10 is switched to the first connection state, and switching valve 20 is switched to the third connection state. Thus, as... Figure 2 As shown by the thick lines, a flow path is formed, consisting of a flow path section 120 and a sample ring 130. At this time, the flow path section 120 is equipped with piping 121 to 124. In this state, the pump 140 operates to direct the sample within the flow path section 120 towards... Figure 2 Press in the direction indicated by the black arrow. In this case, as... Figure 2 As indicated by the blank arrow in the middle, the sample is being compressed.

[0042] Specifically, the sample stored in tank 110 is drawn into pipe 121 through filter 101. The sample drawn into pipe 121 is then introduced into sample ring 130 via ports 11 and 12 of switching valve 10, pipe 122, ports 21 and 22 of switching valve 20, and inlet port 131 of sample ring 130. The sample introduced into sample ring 130 is then discharged from outlet port 132 of sample ring 130 and returned to tank 110 via ports 25 and 26 of switching valve 20, pipe 123, ports 14 and 13 of switching valve 10, pipe 124, and filter 102.

[0043] After that, as Figure 3 As shown, switching valve 10 is switched to the second connection state, while switching valve 20 remains in the third connection state. Thus, as... Figure 3 As shown by the thick lines, a flow path is formed, consisting of a flow path section 120 and a sample ring 130. At this time, the flow path section 120 is equipped with piping 121-125. In this state, the pump 140 operates to direct the sample within the flow path section 120 towards... Figure 3 Press in the direction indicated by the black arrow. In this case, as... Figure 3 As indicated by the blank arrow in the middle, the sample is being compressed.

[0044] Specifically, the sample stored in tank 110 is drawn into pipe 124 through filter 102. The sample drawn into pipe 124 is then introduced into sample ring 130 via ports 13 and 12 of switching valve 10, pipe 122, ports 21 and 22 of switching valve 20, and inlet port 131 of sample ring 130. The sample introduced into sample ring 130 is then discharged from outlet port 132 of sample ring 130 and returned to tank 110 via ports 25 and 26 of switching valve 20, pipe 123, ports 14 and 15 of switching valve 10, pipe 125, ports 16 and 11 of switching valve 10, pipe 121, and filter 101.

[0045] The connection state of switching valve 10 switches between the first connection state and the second connection state at regular intervals. Therefore, Figure 2 cyclical actions and Figure 3 The cyclic operation switches at regular intervals. As a result, the orientation of the samples passing through filters 101 and 102 is switched at regular intervals, and the samples stored in tank 110 are circulated through flow path 120 and sample ring 130.

[0046] After the sample is introduced into the sample loop 130, the sample is supplied to the vial 160. When the sample is supplied to the vial 160, the sample circulation is stopped. Figure 4 This diagram illustrates an example of the sample supply operation to vial 160. (See diagram for example.) Figure 4 As shown, during the sample supply operation to vial 160, switching valve 20 is switched to the fourth connection state, and switching valve 30 is switched to the fifth connection state. Thus, as... Figure 4 As shown by the thick line, pump 150 and vial 160 are connected via... Figure 4 The flow path connections are shown in medium-thick lines. Specifically, Figure 4 The connection flow path includes ports 23 and 22 of switching valve 20, sample ring 130, ports 25 and 24 of switching valve 20, and ports 31 and 32 of switching valve 30.

[0047] In this state, pump 150 performs a sample delivery operation. As a result, the sample stored in sample ring 130 is discharged from outlet port 132 and supplied to any one of vials 160 via ports 25 and 24 of switching valve 20 and ports 31 and 32 of switching valve 30. Consequently, the sample is stored in vial 160.

[0048] exist Figure 4 After the sample supply to vial 160 is completed, the sample supply to the analytical apparatus 200 is carried out. Figure 5 and Figure 6 This diagram illustrates an example of the sample supply operation to the analytical apparatus 200. (See diagram for example.) Figure 5As shown, when the sample is supplied to the analysis apparatus 200, the switching valve 40 is switched to the seventh connection state. Thus, as... Figure 5 As shown in the thick lines, the injection port 180 is connected to the analytical flow path within the analytical apparatus 200 via ports 41 and 42 of the switching valve 40. In this state, the metrology unit 170 uses a sampling needle to collect a sample from the vial 160 and ejects the collected sample to the injection port 180. Thus, the sample ejected to the injection port 180 is supplied to the analytical flow path.

[0049] After the sample is supplied to the analytical flow path within the analytical apparatus 200, such as Figure 6 As shown, switching valve 40 is switched to the 8th connection state. Thus, the mobile phase container 210 of the analysis device 200 is connected to the detector 240 via... Figure 6 The flow path connection is shown in medium-thick lines. This flow path includes the analysis flow path. Specifically, Figure 6 The connection path includes pump 220, ports 42 and 43 of switching valve 40, and analysis column 230.

[0050] In this state, pump 220 performs a mobile phase compression operation. The mobile phase stored in mobile phase container 210 is thus compressed, passed through ports 43 and 42 of switching valve 40, and introduced into analytical column 230 along with the sample supplied to the analytical flow path. The sample, having passed through analytical column 230 with the mobile phase, is separated into various components and detected by detector 240.

[0051] (3) Effects

[0052] In the online sampler 100 of this embodiment, the sample stored in the tank 110 is circulated through the flow path 120. The sample flowing through the flow path 120 is introduced into the interior of the sample ring 130 through the inlet port 131, and the sample introduced into the interior of the sample ring 130 is exported back to the flow path 120 through the outlet port 132. In this case, the sample introduced into the interior of the sample ring 130 can be sampled.

[0053] Here, the two ends of the flow path 120 are disposed within the tank 110, and filters 101 and 102 are respectively installed at both ends. Therefore, even if the sample has a slurry-like consistency containing both liquid and solid components, the solid components are removed from the sample by the filter 101 or filter 102. Thus, it is prevented that the solid components of the sample are introduced into the sample ring 130.

[0054] Furthermore, the orientation of the sample passing through filters 101 and 102 is switched between the first connection state and the second connection state by switching valve 10. According to this structure, whenever the orientation of the sample is switched, the solid components of the sample captured by filters 101 and 102 are flushed away from the surfaces of filters 101 and 102 by the flow of the sample. This reduces the frequency of clogging of filters 101 and 102 and more effectively prevents solid components of the sample from mixing into the interior of the flow path 120. As a result, sample sampling can be performed appropriately.

[0055] Specifically, the switching valve 10 has ports 11 to 16. Additionally, the flow path 120 includes pipes 121 to 125. One end of pipe 121 is connected to port 11, and the other end of pipe 121 has a filter 101 installed inside the container 110. Pipe 122 is connected between the inlet port 131 and port 12 of the sample ring 130. Pipe 123 is connected between the outlet port 132 and port 14 of the sample ring 130. One end of pipe 124 is connected to port 13, and the other end of pipe 124 has a filter 102 installed inside the container 110. Pipe 125 is connected between ports 15 and 16.

[0056] In the first connected state of the switching valve 10, ports 11 and 12, 13 and 14, and 15 and 16 are connected. In the second connected state of the switching valve 10, ports 12 and 13, 14 and 15, and 16 and 11 are connected. In this case, the orientation of the sample passing through filters 101 and 102 can be switched with a simple structure.

[0057] Within the flow path 120, the sample is pressurized by the pump 140. Therefore, even when the sample is in a slurry state, the sample stored in the tank 110 can be easily circulated through the flow path 120.

[0058] The switching valve 20 can switch between a third flow path state and a fourth flow path state. In the third flow path state, the sample ring 130 is inserted into the flow path section 120. The sample is then introduced into the sample ring 130. In the fourth flow path state, the sample ring 130 is inserted between the pump 150 and the vial 160. In this state, the pump 150 performs a pressurization operation, pressurizing the sample introduced into the sample ring 130, and the pressurized sample is stored in the vial 160. In this case, the sample introduced into the sample ring 130 can be sampled into the vial 160 with a simple structure.

[0059] The sample stored in vial 160 is collected by metering unit 170 and supplied to analytical apparatus 200. In this case, the sample can be easily supplied to analytical apparatus 200.

[0060] 2. Second Implementation Method

[0061] (1) Structure of the online sampler

[0062] Regarding the online sampler 100 of the second embodiment of the present invention, the differences from the online sampler 100 of the first embodiment will be explained. Figure 7 This is a diagram illustrating the structure of the online sampler 100 according to the second embodiment of the present invention. Figure 7 As shown, the online sampler 100 of this embodiment does not include switching valves 20 and 30 or pump 150. Therefore, port 44 of switching valve 40 is connected to a waste liquid device (not shown) instead of port 33 of switching valve 30.

[0063] Additionally, the online sampler 100 includes a flow vial 190 for temporary sample storage, replacing the sample loop 130. The flow vial 190 is an example of a sample inlet. An inlet port 191 for introducing the sample into the flow vial 190 and an outlet port 192 for discharging the sample from the flow vial 190 are formed on its outer peripheral surface. The other end of the piping 122 is connected to the inlet port 191 of the flow vial 190, instead of to port 21 of the switching valve 20. The other end of the piping 123 is connected to the outlet port 192 of the flow vial 190, instead of to port 26 of the switching valve 20.

[0064] (2) Operation of the online sampler

[0065] Figure 8 and Figure 9 This diagram illustrates an example of the circulation process of a sample stored in container 110. During the sample circulation process, as... Figure 8 As shown, switching valve 10 is switched to the first connection state. Therefore, as... Figure 8 As shown by the thick lines, a flow path is formed, consisting of a flow path section 120 and a flow vial 190. At this time, the flow path section 120 is equipped with piping 121-124. In this state, the pump 140 operates to direct the sample within the flow path section 120 towards... Figure 8 Press in the direction indicated by the black arrow. In this case, as... Figure 8 As indicated by the blank arrow in the middle, the sample is being compressed.

[0066] Specifically, the sample stored in tank 110 is drawn into piping 121 through filter 101. The sample drawn into piping 121 is then introduced into flow vial 190 via ports 11 and 12 of switching valve 10, piping 122, and inlet port 191 of flow vial 190. The sample introduced into flow vial 190 is then discharged from outlet port 192 of flow vial 190 and returned to tank 110 via piping 123, ports 14 and 13 of switching valve 10, piping 124, and filter 102.

[0067] After that, as Figure 9 As shown, switching valve 10 is switched to the second connection state. Therefore, as... Figure 9 As shown by the thick lines, a flow path is formed, consisting of a flow path section 120 and a flow vial 190. At this time, the flow path section 120 is equipped with piping 121-125. In this state, the pump 140 operates to direct the sample within the flow path section 120 towards... Figure 9 Press in the direction indicated by the black arrow. In this case, as... Figure 9 As indicated by the blank arrow in the middle, the sample is being compressed.

[0068] Specifically, the sample stored in tank 110 is drawn into piping 124 through filter 102. The sample drawn into piping 124 is then introduced into flow vial 190 via ports 13 and 12 of switching valve 10, piping 122, and inlet port 191 of flow vial 190. The sample introduced into flow vial 190 is discharged from outlet port 192 of flow vial 190 and returns to tank 110 via piping 123, ports 14 and 15 of switching valve 10, piping 125, ports 16 and 11 of switching valve 10, piping 121, and filter 101.

[0069] The connection state of switching valve 10 switches between the first connection state and the second connection state at regular intervals. Therefore, Figure 8 cyclical actions and Figure 9 The cyclic operation switches at regular intervals. As a result, the orientation of the samples passing through filters 101 and 102 is switched at regular intervals, and the samples stored in tank 110 are circulated through flow path 120 and flow vial 190.

[0070] During the sample feeding action to vial 160, Figure 8 and Figure 9 The sample circulation process can be stopped or resumed. During the sample supply operation to vial 160, the metrology unit 170 uses a sampling needle to collect the sample from the flow vial 190 and dispenses the collected sample into any one of the vials 160. Thus, the sample is supplied to vial 160. As a result, the sample is stored in vial 160.

[0071] After the sample supply operation to vial 160, the sample supply to the analytical apparatus 200 is performed. The sample supply operation to the analytical apparatus 200 in this embodiment is the same as that in the first embodiment. Figure 5 and Figure 6The sample supply operation to the analytical apparatus 200 is the same. Furthermore, if no sample pretreatment is performed, the sample supply operation to the vial 160 can be omitted. In this case, the online sampler 100 may not include the vial 160. In this configuration, the metrology unit 170 collects the sample from the flow vial 190 and... Figure 5 Similarly, the collected sample is ejected into injection port 180. Then, it is subjected to... Figure 6 The same sample supply operation is performed to the analysis device 200.

[0072] (3) Effects

[0073] In the online sampler 100 of this embodiment, similarly to the first embodiment, the sample stored in the tank 110 is circulated through the flow path section 120. The sample flowing through the flow path section 120 is introduced into the interior of the flow vial 190 via the inlet port 191, and the sample introduced into the flow vial 190 is exported back to the flow path section 120 via the outlet port 192. In this case, the sample introduced into the flow vial 190 can be sampled.

[0074] Here, the two ends of the flow path 120 are disposed within the tank 110, and filters 101 and 102 are respectively installed at both ends. Therefore, even if the sample has a slurry-like consistency containing both liquid and solid components, the solid components are removed from the sample by the filter 101 or filter 102. Thus, it is prevented that the solid components of the sample are introduced into the flow vial 190.

[0075] Furthermore, the orientation of the sample passing through filters 101 and 102 is switched between the first connection state and the second connection state by switching valve 10. According to this structure, whenever the orientation of the sample is switched, the solid components of the sample captured by filters 101 and 102 are flushed away from the surfaces of filters 101 and 102 by the flow of the sample. This reduces the frequency of clogging of filters 101 and 102 and more effectively prevents solid components of the sample from mixing into the interior of the flow path 120. As a result, sample sampling can be performed appropriately.

[0076] The flow vial 190 is inserted into the flow path section 120. The sample introduced into the flow vial 190 is collected by the metering section 170 and supplied to the vial 160 or the analytical device 200. In this case, the sample introduced into the flow vial 190 can be sampled into the vial 160 or supplied to the analytical device 200 with a simple structure.

[0077] 3. Third Implementation Method

[0078] Regarding the online sampler 100 of the third embodiment, the differences from the online sampler 100 of the first embodiment will be explained. Figure 10 This is a diagram illustrating the structure of the online sampler 100 according to the third embodiment of the present invention. Figure 10 As shown, the online sampler 100 of this embodiment does not include the switching valve 30. Therefore, port 44 of the switching valve 40 is connected to a waste liquid device (not shown), rather than to port 33 of the switching valve 30.

[0079] Additionally, the online sampler 100, like in the second embodiment, includes a flow vial 190 for temporary sample storage. Port 24 of the switching valve 20 is connected to the inlet port 191 of the flow vial 190, rather than to port 31 of the switching valve 30. The outlet port 192 of the flow vial 190 is connected, for example, to the aforementioned waste disposal device. The outlet port 192 of the flow vial 190 may also be connected to the tank 110.

[0080] The cyclic operation of the sample in this embodiment is the same as that in the first embodiment. Figure 2 and Figure 3 The cyclic action of the sample is the same. After the sample cyclic action, the sample is supplied to the flow vial 190. When the sample is supplied to the flow vial 190, the sample cyclic action is stopped.

[0081] Figure 11 This diagram illustrates an example of the sample supply operation to the flow vial 190. (See diagram for example.) Figure 11 As shown, when the sample is supplied to the flow vial 190, the switching valve 20 is switched to the fourth connection state. Thus, as... Figure 11 As shown by the thick line, pump 150 and flow vial 190 are connected via... Figure 11 The flow path connections are shown in medium-thick lines. Specifically, Figure 11 The connection flow path includes ports 23 and 22 of the switching valve 20, sample ring 130, and ports 25 and 24 of the switching valve 20.

[0082] In this state, pump 150 performs a sample delivery operation. As a result, the sample stored in sample ring 130 is discharged from outlet port 132 and supplied to flow vial 190 via ports 25 and 24 of switching valve 20 and inlet port 191 of flow vial 190. Consequently, the sample is temporarily stored in flow vial 190. The sample stored in flow vial 190 is discharged to waste liquid device via outlet port 192 or returned to tank 110.

[0083] After the sample is supplied to the flow vial 190, the same sample supply operation to the vial 160 is performed as in the second embodiment. Specifically, the metrology unit 170 uses a sampling needle to collect the sample from the flow vial 190 and ejects the collected sample into any one of the vials 160. Thus, the sample is supplied to the vial 160. As a result, the sample is stored in the vial 160. Afterward, the same sample supply operation to the analytical apparatus 200 is performed as in the first or second embodiment. Furthermore, if the sample in the vial 160 is not pretreated, the sample supply operation to the vial 160 can be omitted. In this case, the online sampler 100 may not include the vial 160.

[0084] 4. Other implementation methods

[0085] In the above embodiment, the pump 140 is inserted into the piping 122 or piping 123 of the flow path section 120, but the embodiment is not limited to this. As long as the sample in the flow path section 120 can be pressurized, the pump 140 can also be inserted into the piping 121 or piping 124 of the flow path section 120, or it can be provided in other parts.

[0086] Furthermore, in the above embodiment, the online sampler 100 is connected to the analysis device 200, but the embodiment is not limited to this. When no sample analysis is being performed, the online sampler 100 may not be connected to the analysis device 200. In this case, the online sampler 100 may not include the metrology unit 170.

[0087] 5. Method

[0088] Those skilled in the art will understand that the above-described exemplary embodiments are specific examples of the following approaches.

[0089] (Item 1) An online sampler of one type, which may include:

[0090] Containers for storing samples;

[0091] The flow path section has a first end and a second end disposed within the container, and circulates the sample stored in the container;

[0092] The first filter is installed at the first end of the flow path section;

[0093] The second filter is installed at the second end of the flow path section;

[0094] The sample inlet has: an inlet port for introducing a sample flowing through the flow path into the interior; and an outlet port for exporting the sample introduced into the interior to the flow path.

[0095] A first pump is used to pressurize the sample flowing through the flow path; and

[0096] The first switching valve is capable of switching between a first connection state and a second connection state. The first connection state is when the sample in the tank is introduced into the flow path section from the first end, and the sample in the flow path section is discharged into the tank from the second end. The second connection state is when the sample in the tank is introduced into the flow path section from the second end, and the sample in the flow path section is discharged into the tank from the first end.

[0097] In this online sampler, the sample stored in the tank is circulated through the flow path. The sample flowing through the flow path is introduced into the sample inlet through the inlet port, and the sample introduced into the sample inlet is exported back to the flow path through the outlet port. In this case, the sample introduced into the sample inlet can be sampled.

[0098] Here, the first and second ends of the flow path are disposed inside the tank, and a first filter and a second filter are respectively installed at the first and second ends. Therefore, even if the sample has a slurry-like consistency containing both liquid and solid components, the solid components are removed from the sample by the first or second filter. Thus, it prevents the solid components of the sample from being introduced into the sample inlet.

[0099] Furthermore, the orientation of the sample passing through the first and second filters is switched between the first and second connection states via a first switching valve. According to this structure, whenever the sample orientation is switched, the solid components of the sample captured by the first and second filters are flushed away from the surfaces of the first and second filters by the sample flow. This reduces the frequency of clogging of the first and second filters and more effectively prevents solid components of the sample from mixing into the interior of the flow path. As a result, proper sampling of the sample is possible.

[0100] (Item 2) In the online sampler described in Item 1, the first switching valve may have a first port, a second port, a third port, a fourth port, a fifth port, and a sixth port.

[0101] The flow path section includes:

[0102] The first flow path section has one end connected to the first port, and the other end is equipped with the first filter inside the tank;

[0103] The second flow path is connected between the inlet port and the second port of the sample inlet section;

[0104] The third flow path is connected between the outlet port of the sample inlet and the fourth port;

[0105] A fourth flow path section, one end of which is connected to the third port, and the other end of which is fitted with the second filter inside the tank; and

[0106] The fifth flow path is connected between the fifth port and the sixth port.

[0107] In the first connection state, connections are established between the first port and the second port, between the third port and the fourth port, and between the fifth port and the sixth port.

[0108] In the second connection state, the second port is connected to the third port, the fourth port is connected to the fifth port, and the sixth port is connected to the first port.

[0109] In this case, the orientation of the sample passing through the first filter and the second filter can be switched with a simple structure.

[0110] (Item 3) In the online sampler described in Item 2, the first pump may be disposed in the second flow path section.

[0111] In this case, the sample can be efficiently pressurized and fed through the flow path.

[0112] (Item 4) In the online sampler described in Item 2, the first pump may be located in the third flow path section.

[0113] In this case, the sample can be efficiently pressurized and fed through the flow path.

[0114] (Item 5) The online sampler in any one of items 1 to 4 may further include:

[0115] The second pump is used to pressurize and introduce the sample into the sample inlet section;

[0116] A vial for storing the sample pressurized by the second pump; and

[0117] The second switching valve is capable of switching between a third flow path state and a fourth flow path state. The third flow path state is when the sample inlet is inserted into the flow path, and the fourth flow path state is when the sample inlet is inserted between the second pump and the vial.

[0118] In this case, the sample introduced into the sample inlet can be sampled into a vial with a simple structure.

[0119] (Item 6) The online sampler described in Item 5 may further include:

[0120] The metrology unit is used to collect samples from the vials and supply them to the analytical apparatus.

[0121] In this case, the sample can be easily supplied to the analytical apparatus.

[0122] (Item 7) In the online sampler described in Item 5 or Item 6, the sample inlet may be a sample ring.

[0123] In this case, the sample can be introduced into the sample introduction section with a simple structure, and the sample introduced into the sample introduction section can be sampled into a vial.

[0124] (Item 8) The online sampler in any one of items 1 to 4 may further include:

[0125] The metrology unit is used to collect samples from the sample inlet and supply them to a specified vial or analytical device.

[0126] The sample inlet can be inserted into the flow path.

[0127] In this case, the sample introduced into the sample inlet can be sampled into a vial with a simple structure, or the sample introduced into the sample inlet can be supplied to the analytical device.

[0128] (Item 9) In the online sampler described in Item 8, the sample inlet may be a flow vial.

[0129] In this case, the sample can be introduced into the sample introduction section with a simple structure, and the sample introduced into the sample introduction section can be sampled into a vial, or the sample introduced into the sample introduction section can be supplied to the analytical device.

Claims

1. An on-line sampler comprising: a tank that stores a sample; a flow path section that has a first end portion and a second end portion disposed in the tank and circulates the sample stored in the tank; a first filter that is installed at the first end portion of the flow path section; a second filter that is installed at the second end portion of the flow path section; a sample introduction section that has: an introduction port for introducing the sample flowing through the flow path section into the inside; and an outlet port for leading the sample introduced into the inside to the flow path section; a first pump for pressurizing and feeding the sample flowing through the flow path section; and a first switching valve that is switchable between a first connection state in which the sample in the tank is introduced from the first end portion to the flow path section and the sample in the flow path section is led from the second end portion to the tank, and a second connection state in which the sample in the tank is introduced from the second end portion to the flow path section and the sample in the flow path section is led from the first end portion to the tank.

2. The on-line sampler according to claim 1, wherein the first switching valve has a first port, a second port, a third port, a fourth port, a fifth port, and a sixth port, the flow path section includes: a first flow path section whose one end portion is connected to the first port and whose other end portion is installed with the first filter in the tank; a second flow path section that is connected between the introduction port of the sample introduction section and the second port; a third flow path section that is connected between the outlet port of the sample introduction section and the fourth port; a fourth flow path section whose one end portion is connected to the third port and whose other end portion is installed with the second filter in the tank; and a fifth flow path section that is connected between the fifth port and the sixth port, in the first connection state, the first port and the second port, the third port and the fourth port, and the fifth port and the sixth port are connected, in the second connection state, the second port and the third port, the fourth port and the fifth port, and the sixth port and the first port are connected.

3. The on-line sampler according to claim 2, wherein the first pump is provided in the second flow path section.

4. The on-line sampler according to claim 2, wherein the first pump is provided in the third flow path section.

5. The on-line sampler according to any one of claims 1 to 3, further comprising: a second pump for pressurizing and feeding the sample introduced into the sample introduction section; a vial for storing the sample pressurized and fed by the second pump; and a second switching valve that is switchable between a third flow path state in which the sample introduction section is inserted in the flow path section, and a fourth flow path state in which the sample introduction section is inserted between the second pump and the vial.

6. The on-line sampler according to claim 5, further comprising: a metering section for collecting the sample from the vial and supplying it to an analysis device. ​ ​ ​ ​ 7. The on-line sampler according to claim 5, wherein the sample introduction section is a sample loop.

8. The on-line sampler according to any one of claims 1 to 3, further comprising: a metering section for collecting a sample from the sample introduction section and supplying it to a prescribed vial or analysis device, the sample introduction section being inserted in the flow path section.

9. The on-line sampler according to claim 8, wherein the sample introduction section is a flow vial. ​ ​

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