System flow path for solid phase extraction and method of use
By designing the flow path of the solid-phase extraction system and using components such as rotary valves and sample loaders, fully automatic negative pressure sample loading and normal pressure collection are achieved, solving the clogging and sealing problems in the processing of large-volume and dirty wastewater samples, and improving experimental efficiency and success rate.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- BEIJING LABTECH
- Filing Date
- 2023-11-13
- Publication Date
- 2026-04-17
AI Technical Summary
Existing solid phase extraction instruments suffer from problems such as easy damage to liquid path components, easy blockage of pipelines, cross-contamination, and poor sealing when processing large-volume and dirty wastewater samples, resulting in biased experimental results and low efficiency.
A solid-phase extraction system flow path was designed, employing a rotary valve, sample loader, membrane adapter, and gas path system to achieve fully automated negative pressure sample loading and atmospheric pressure collection. The system integrates gas and liquid paths and includes a spray cleaning function. By selecting the flow path of the sample loader and switching the flow path of the liquid pump, the problems of blockage and sealing are solved, thus improving the success rate of experiments.
It has achieved online filtration and full-process automation of dirty sewage samples, improved the success rate of experiments and sample recovery rate, and solved the problems of clogging, poor sealing and cross-contamination in the existing technology, thus realizing full-process automation.
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Figure CN117323697B_ABST
Abstract
Description
Technical Field
[0001] This invention relates to a system flow path for solid-phase extraction and its application method. Background Technology
[0002] Solid-phase extraction (SPE) technology, as an important component of current sample pretreatment techniques, has wide applications in many fields such as food safety, pharmaceuticals, and environmental analysis. The SPE process includes column / membrane activation, sample loading, sample vial cleaning, rinsing, and elution steps.
[0003] Almost all existing fully automated solid-phase extraction (SPE) instruments employ positive pressure loading, using various types of pumps as the power source for sample passage through the column / membrane. Manual or semi-automatic SPE instruments mostly achieve negative pressure loading by using vacuum pumps to create negative pressure. SPE is a widely used sample pretreatment method, with loading volumes ranging from a few milliliters to several liters. Environmental water samples mainly include river water, lake water, groundwater, drinking water, seawater, and industrial wastewater. Different water bodies exhibit matrix effects; for example, suspended particles, colloids, silt, and algae in surface water can all affect the efficiency of pretreatment methods. Using fully automated syringe pumps or rotary valves for sample loading often leads to problems such as easy damage to liquid path components, easy blockage of pipelines and rotary valves, and cross-contamination, resulting in functional failures or inaccurate test results.
[0004] Current solid-phase extraction (SPE) collection processes employ either negative or positive pressure methods. For manual or semi-automatic instruments, a vacuum pump typically creates negative pressure within the bottle to allow the eluent to flow from the column / membrane to the collection bottle. For fully automated instruments, a one-way valve can be introduced to reduce pressure and open, allowing the collection liquid to enter. However, excessively low negative pressure can cause the collection liquid to boil violently, resulting in the loss of the target substance. Furthermore, the one-way valve requires routine cleaning and maintenance; if contaminated samples are loaded and particles pass through the column / membrane into the one-way valve, it can malfunction and leak. For positive pressure collection processes in fully automated, semi-automatic, and manual SPE instruments, a tight seal of the column / membrane is essential to prevent leakage and eluent collection. While structures are designed to ensure this seal, these are complex and increase the risk of experimental failure. Summary of the Invention
[0005] The purpose of this invention is to provide a system flow path for solid-phase extraction and its application method, enabling a solid-phase extraction pretreatment process that is more suitable for large-volume and dirty wastewater samples. Specifically, it includes fully automated solvent transfer, negative pressure sample loading, and normal pressure collection, as well as applications for special needs such as spraying sample bottles, online filtration, and online dehydration during the processing.
[0006] To achieve the above objectives, the technical solution adopted by the present invention is as follows:
[0007] A solid-phase extraction system flow path is characterized by: a rotary valve having several solvent inlet ports, a solvent outlet port, and a waste liquid port arranged circumferentially on its upper circumference; a pump inlet port being arranged below the rotary valve; one end of the pump inlet port being connected to an injection pump; the other end of the pump inlet port being connected to a common channel; the common channel being connected to one of the solvent inlet ports, the solvent outlet port, and the waste liquid port through the rotation of a selection channel; the solvent inlet port being connected to a solvent bottle; the solvent outlet port being connected to a sample loader; and a gas path system being connected to the pipeline between the rotary valve and the sample loader.
[0008] The sample loader has several channels and includes a valve core and a valve body. The sample loader controls the connection of the channels by rotating the valve core.
[0009] A membrane adapter is provided below the sample loader. An upper port is provided at the top of the collection dock, which is connected to the membrane adapter. A lower port is provided at the bottom of the collection dock, which is connected to the dehydration device and the collection bottle. An outlet and an inlet are provided on the collection dock, which are connected to the flow path switching system. A pressure balance port is also provided on the collection dock, which is connected to the outside to balance the pressure inside the collection bottle.
[0010] The top of the valve body is connected to the sample bottle, and a spray needle is also provided at the top of the valve body and placed inside the sample bottle. A guide tube is also provided at the bottom of the valve body.
[0011] The valve body is provided with longitudinal channels, namely a main solvent channel, a spray channel and a sample flow channel. The bottom end of the main solvent channel is provided with a solvent interface. The pipeline between the solvent interface and the solvent outlet port is connected to the gas circuit system. The valve body is also provided with transverse channels, namely an activation solvent channel and a cleaning solvent channel. The main solvent channel is connected to the activation solvent channel and the cleaning solvent channel respectively. The spray channel is connected to the spray needle. The sample flow channel is connected to the guide tube.
[0012] The valve core is disposed within the valve body. The valve core is provided with a sample loading channel, a cleaning channel, and an activation channel. When the valve core is rotated to the open position, the sample loading channel rotates to a position coaxially connected with the sample flow channel, and the spray channel, the cleaning channel, the cleaning solvent channel, and the main solvent channel are connected. When the valve core is rotated to the closed position, the sample loading channel rotates to a position not connected with the sample flow channel, and the main solvent channel, the activation solvent channel, the activation channel, and the sample flow channel are connected.
[0013] The solid-phase extraction system flow path includes: the gas path system includes an on / off valve, a pressure regulating valve and a gas source, and the pressure regulating valve and the on / off valve are sequentially installed at the top of the gas source for regulating the gas pressure and opening / closing the gas pipeline.
[0014] The solid-phase extraction system flow path includes: a liquid level sensor installed in the membrane adapter to monitor the liquid level; an extraction membrane placed in the membrane adapter; and a filter medium added to the extraction membrane.
[0015] The solid-phase extraction system flow path includes: a flow path switching system comprising a speed control valve, a liquid pump, a selection valve, a waste liquid selection valve, an aqueous waste liquid tank, and an organic waste liquid tank; the C-end of the speed control valve is connected to the liquid outlet; the NC-end of the speed control valve is connected to the inlet of the liquid pump; the outlet of the liquid pump is connected to the C-end of the selection valve; the NC-end of the selection valve is connected to the liquid inlet; the NO-end of the selection valve is connected to the C-end of the waste liquid selection valve; the NO-end of the waste liquid selection valve is connected to the aqueous waste liquid tank; and the NC-end of the waste liquid selection valve is connected to the organic waste liquid tank.
[0016] A method for applying a system flow path for solid-phase extraction, characterized in that:
[0017] When the system requires activation, rotate the selector channel of the rotary valve to one of the solvent inlet ports. The syringe pump draws the activation solvent from the solvent bottle. Then rotate the selector channel to the solvent outlet port. The syringe pump pushes out the activation solvent, which enters the main solvent channel from the solvent inlet. At this time, the valve core is in the closed state. The sample loading channel and the sample flow channel are not connected. The spray channel and the cleaning solvent channel are closed by the valve core. The activation solvent can only flow into the activation solvent channel and the activation channel, and then into the lower half of the sample flow channel. Finally, it flows into the membrane adapter through the guide tube to activate the extraction membrane. The activation solvent passes through the filter medium and the extraction membrane into the collection dock. The activation solvent flows from the upper port through the outlet and enters the speed control valve, the pump, and the selector valve in sequence. It flows out from the NO end of the selector valve and finally enters the water waste tank or the organic waste tank through the waste liquid selector valve according to the waste liquid type, so as to realize the classified collection of waste liquid.
[0018] When the system requires rinsing, the process is the same as the activation process described above, and a solvent is selected to clean the extraction membrane.
[0019] When the system requires sample loading, the valve core is in the open state, the sample loading channel and the sample flow channel are connected, and the sample flows out from the sample bottle into the membrane adapter. At this time, the rotary valve is in the closed position. Although the solvent interface, the main solvent channel and the spray channel are connected, the sample will not flow out from the spray channel and be lost. The liquid remaining in the pipeline is blown back into the sample bottle through the gas system. The liquid level sensor monitors the liquid level of the membrane adapter and controls the opening and closing of the valve core to prevent the sample from overflowing from the membrane adapter. Dirt particles in the sample are intercepted by the filter medium, and the effective substances in the sample are adsorbed by the extraction membrane. The waste liquid enters the collection dock. The waste liquid flows from the upper port through the outlet and sequentially enters the speed control valve, the pump, and the selection valve. It flows out from the NO end of the selection valve and finally enters the water waste tank through the NO end of the waste liquid selection valve according to the waste liquid type.
[0020] When the system requires cleaning sample vials, the selection channel of the rotary valve is rotated to one of the solvent inlet ports. The syringe pump draws the cleaning solvent from the solvent vial. Then, the selection channel is rotated to the solvent outlet port, and the valve core is in the open state. The gas path system is then opened, and the cleaning solvent and gas enter together from the solvent interface, flowing sequentially through the main solvent channel, the cleaning solvent channel, the cleaning channel, and finally into the spray needle from the spray channel to clean the sample vials. After the cleaning solvent has finished spraying the sample vials, it flows from the sample flow channel through the guide tube into the membrane adapter. The cleaning solvent passes through the filter medium and the extraction membrane and enters the collection dock. The cleaning solvent flows from the upper port through the liquid outlet, sequentially into the speed control valve, the liquid pump, and the selection valve, and flows out from the NO end of the selection valve. Finally, depending on the waste liquid type, it enters the aqueous waste liquid tank or the organic waste liquid tank through the waste liquid selection valve, achieving waste liquid classification and collection.
[0021] When the system requires elution, the selector channel of the rotary valve is rotated to one of the solvent inlet ports. The syringe pump draws the elution solvent from the solvent bottle. Then, the selector channel is rotated to the solvent outlet port, and the syringe pump ejects the elution solvent. The valve core is closed, and the elution solvent enters the main solvent channel from the solvent inlet. The elution solvent can only flow into the activation solvent channel and the activation channel, then into the lower half of the sample flow channel, and finally flows through the guide tube to the membrane adapter to extract the adsorbed substances on the extraction membrane. The sample is eluted, and the elution solvent passes through the filter medium and the extraction membrane, and enters the collection port. The cleaning solvent flows from the upper port through the liquid outlet, and sequentially enters the speed control valve, the liquid pump, and the selection valve. It enters the liquid inlet from the NC end of the selection valve, flows out from the lower port, passes through the dehydration device, and finally enters the collection bottle, realizing online dehydration. If the elution solvent needs to clean the sample bottle during the elution process, the sample bottle cleaning process can be followed. However, the final eluent needs to pass through the NC end of the selection valve to be collected in the collection bottle.
[0022] The beneficial effects of this invention are:
[0023] (1) The system flow path and application method of the present invention for solid phase extraction are used to load samples by selecting the flow channel of the sample loader. The sample flow channel has a large aperture, and dirty samples can be directly loaded. Online filtration is performed without the need for pre-filtration, which solves the problem of dirty samples clogging the system.
[0024] (2) This invention achieves fully automatic negative pressure sample loading and normal pressure collection by switching the flow path of the liquid pump and solenoid valve and selecting the collection docking channel. It solves the problems of poor sealing under positive pressure, failure of one-way valve sealing and boiling under negative pressure during the fully automatic collection process, and improves the success rate of the experiment.
[0025] (3) This invention integrates the gas path and the liquid path, and at the same time achieves the function of spraying and cleaning the sample bottle through the spray needle, ensuring complete sample loading, solving the problem of sample residue in the sample bottle, thereby improving the sample recovery rate;
[0026] (4) The sample loader of the present invention can be detached and ultrasonically cleaned, which solves the problems of sample residue, blockage and cross-contamination of the finished rotary valve in the existing method;
[0027] (5) This invention solves the problem that existing negative pressure loading methods cannot automatically adjust the flow rate;
[0028] (6) This invention solves the problem that existing methods cannot remove water online, realizes full-process automation, and improves experimental efficiency. Attached Figure Description
[0029] Figure 1 This is a schematic diagram of the flow path for solid-phase extraction.
[0030] Figure 2 This is a structural diagram showing the sample loader in the off state.
[0031] Figure 3 A structural diagram showing the sample loader in the open state.
[0032] Figure labeling: 1-Rotary valve; 101-Pump inlet port; 102-Solvent inlet port; 103-Solvent outlet port; 104-Waste liquid port; 105-Common channel; 106-Selection channel; 2-Solvent bottle; 3-Injection pump; 4-Gas system; 401-On / off valve; 402-Pressure regulating valve; 403-Gas source; 5-Sample bottle; 6-Spray needle; 7-Sample loader; 8-Valve core; 801-Sample loading channel; 802-Cleaning channel; 803-Activation channel; 9-Valve body; 901-Solvent interface; 902-Activation solvent channel; 903-Main solvent channel; 904-Cleaning solvent channel ; 905-Spray channel; 906-Sample flow channel; 907-Guide tube; 10-Level sensor; 11-Membrane adapter; 1101-Extraction membrane; 1102-Filter medium; 12-Collection docking point; 1201-Upper port; 1202-Lower port; 1203-Outlet; 1204-Inlet; 1205-Pressure balance port; 13-Water removal device; 14-Collection bottle; 15-Flow path switching system; 1501-Speed control valve; 1502-Liquid pump; 1503-Selection valve; 1504-Waste liquid selection valve; 1505-Aqueous waste liquid tank; 1506-Organic waste liquid tank. Detailed Implementation
[0033] like Figure 1 The diagram illustrates a solid-phase extraction system flow path. A rotary valve 1 has several solvent inlet ports 102, a solvent outlet port 103, and a waste liquid port 104 arranged circumferentially on its upper circumference. Below the rotary valve 1 is a pump inlet port 101. One end of the pump inlet port 101 is connected to a syringe pump 3, and the other end is connected to a common channel 105. The common channel 105 is also connected to one of the solvent inlet ports 102, the solvent outlet port 103, and the waste liquid port 104 via the rotation of a selection channel 106. The solvent inlet port 102 is connected to a solvent bottle 2, and the solvent outlet port 103 is connected to a sample loader 7. A gas path system 4 is connected to the pipeline between the rotary valve 1 and the sample loader 7.
[0034] The gas system 4 includes an on / off valve 401, a pressure regulating valve 402, and a gas source 403. The pressure regulating valve 402 and the on / off valve 401 are sequentially installed at the top of the gas source 403 to regulate the gas pressure and open / close the gas pipeline.
[0035] The sample loader 7 has several channels and includes a valve core 8 and a valve body 9. The sample loader 7 controls the connection of the channels by rotating the valve core 8.
[0036] The top end of the valve body 9 is connected to the sample bottle 5. The top end of the valve body 9 is also provided with a spray needle 6, which is placed inside the sample bottle 5. The bottom end of the valve body 9 is also provided with a guide tube 907.
[0037] A membrane adapter 11 is provided below the sample loader 7. A liquid level sensor 10 is provided inside the membrane adapter 11 to monitor the liquid level. An extraction membrane 1101 is placed inside the membrane adapter 11, and a filter medium 1102 is added to the extraction membrane 1101.
[0038] The top of the collection docking point 12 is provided with an upper port 1201, which is connected to the membrane adapter 11. The bottom of the collection docking point 12 is provided with a lower port 1202, which is connected to the water removal device 13 and the collection bottle 14. The collection docking point 12 is provided with an outlet 1203 and an inlet 1204, which are connected to the flow path switching system 15. The collection docking point 12 is also provided with a pressure balance port 1205, which is connected to the outside to balance the pressure inside the collection bottle 14.
[0039] The flow path switching system 15 includes a speed control valve 1501, a liquid pump 1502, a selection valve 1503, a waste liquid selection valve 1504, an aqueous waste liquid tank 1505, and an organic waste liquid tank 1506. The C-end of the speed control valve 1501 is connected to the outlet 1203, the NC-end of the speed control valve 1501 is connected to the inlet of the liquid pump 1502, the outlet of the liquid pump 1502 is connected to the C-end of the selection valve 1503, the NC-end of the selection valve 1503 is connected to the inlet 1204, the NO-end of the selection valve 1503 is connected to the C-end of the waste liquid selection valve 1504, the NO-end of the waste liquid selection valve 1504 is connected to the aqueous waste liquid tank 1505, and the NC-end of the waste liquid selection valve 1504 is connected to the organic waste liquid tank 1506.
[0040] like Figures 2 to 3As shown, the valve body 9 has longitudinal channels including a main solvent channel 903, a spray channel 905, and a sample flow channel 906. The gas system 4 is connected to the pipeline between the solvent interface 901 and the solvent outlet port 103 to supply gas to the pipeline. The solvent interface 901 is provided at the bottom of the main solvent channel 903. The valve body 9 also has transverse channels including an activation solvent channel 902 and a cleaning solvent channel 904. The main solvent channel 903 is connected to the activation solvent channel 902 and the cleaning solvent channel 904 respectively. The spray channel 905 is connected to the spray needle 6. The sample flow channel 906 is connected to the guide tube 907.
[0041] The valve core 8 is disposed within the valve body 9. The valve core 8 is provided with a sample loading channel 801, a cleaning channel 802, and an activation channel 803. When the valve core 8 is rotated to the open position, the sample loading channel 801 rotates to a position coaxially connected with the sample flow channel 906, and the spray channel 905, the cleaning channel 802, the cleaning solvent channel 904, and the main solvent channel 903 are connected. When the valve core 8 is rotated to the closed position, the sample loading channel 801 rotates to a position not connected with the sample flow channel 906, and the main solvent channel 903, the activation solvent channel 902, the activation channel 803, and the sample flow channel 906 are connected.
[0042] A method for applying a system flow path for solid-phase extraction, characterized in that:
[0043] When the system requires activation, rotate the selector channel 106 of the rotary valve 1 to one of the solvent inlet ports 102. The syringe pump 3 draws the activation solvent from the solvent bottle 2. Then rotate the selector channel 106 to the solvent outlet port 103. The syringe pump 3 pushes out the activation solvent, which enters the main solvent channel 903 from the solvent inlet 901. At this time, the valve core 8 is in the closed state. The sample loading channel 801 and the sample flow channel 906 are not connected. The spray channel 905 and the cleaning solvent channel 904 are closed by the valve core 8. The activation solvent can only flow into the activation solvent channel 902 and the activation channel 8. 03, then flows into the lower half of the sample flow channel 906, and finally flows into the membrane adapter 11 through the guide tube 907 to activate the extraction membrane 1101. The activation solvent passes through the filter medium 1102 and the extraction membrane 1101 into the collection dock 12. The activation solvent flows from the upper port 1201 through the outlet 1203, and sequentially enters the speed control valve 1501, the pump 1502, and the selection valve 1503. It flows out from the NO end of the selection valve 1503, and finally enters the water waste tank 1505 or the organic waste tank 1506 through the waste liquid selection valve 1504 according to the waste liquid type, so as to realize the classified collection of waste liquid.
[0044] When the system requires rinsing, the process is the same as the activation process described above, and a solvent is selected to clean the extraction membrane 1101.
[0045] When the system requires sample loading, the valve core 8 is in the open state, and the sample loading channel 801 and the sample flow channel 906 are connected. The sample flows out of the sample bottle 5 and into the membrane adapter 11. At this time, the rotary valve 1 is in the closed position. Although the solvent interface 901, the main solvent channel 903, and the spray channel 905 are connected, the sample will not flow out of the spray channel 905 and be lost. The liquid remaining in the pipeline is blown back into the sample bottle 5 through the gas system 4. The liquid level sensor 10 monitors the liquid level of the membrane adapter 11 and controls the opening and closing of the valve core 8 to prevent the sample from being lost. Sample overflows from membrane adapter 11, contaminant particles in the sample are intercepted by the filter medium 1102, and effective substances in the sample are adsorbed by the extraction membrane 1101. Waste liquid enters the collection dock 12 and flows from the upper port 1201 through the outlet 1203, sequentially entering the speed control valve 1501, the pump 1502, and the selection valve 1503. It flows out from the NO end of the selection valve 1503 and finally enters the water system waste liquid tank 1505 through the NO end of the waste liquid selection valve 1504 according to the waste liquid type. During this process, the parameters of the speed control valve 1501 can be changed to control the system flow rate.
[0046] When the system requires cleaning sample vials, rotate the selection channel 106 of the rotary valve 1 to one of the solvent inlet ports 102. The syringe pump 3 draws cleaning solvent from the solvent vial 2. Then rotate the selection channel 106 to the solvent outlet port 103, opening the valve core 8. The gas path system 4 is then opened, allowing the cleaning solvent and gas to enter through the solvent inlet 901. The gas flows sequentially through the main solvent channel 903, the cleaning solvent channel 904, the cleaning channel 802, and finally into the spray needle 6 through the spray channel 905 to clean the sample vials 5. The cleaning solvent spraying is complete. After the sample vial 5 is inserted, the cleaning solvent enters the membrane adapter 11 through the sample flow channel 906 and the guide tube 907. The cleaning solvent passes through the filter medium 1102 and the extraction membrane 1101 and enters the collection dock 12. The cleaning solvent flows from the upper port 1201 through the liquid outlet 1203 and sequentially enters the speed control valve 1501, the liquid pump 1502, and the selection valve 1503. It flows out from the NO end of the selection valve 1503 and finally enters the aqueous waste liquid tank 1505 or the organic waste liquid tank 1506 through the waste liquid selection valve 1504 according to the waste liquid type, so as to realize the classified collection of waste liquid.
[0047] When the system requires elution, the selection channel 106 of the rotary valve 1 is rotated to one of the solvent inlet ports 102. The syringe pump 3 draws the elution solvent from the solvent bottle 2. Then, the selection channel 106 is rotated to the solvent outlet port 103, and the syringe pump 3 pushes out the elution solvent. The valve core 8 is in the closed state, and the elution solvent enters the main solvent channel 903 from the solvent interface 901. The elution solvent can only flow into the activation solvent channel 902 and the activation channel 803, then into the lower half of the sample flow channel 906, and finally flows into the membrane adapter 11 through the guide tube 907 to elute the substances adsorbed on the extraction membrane 1101. The elution solvent passes through the filter medium 1102 and the extraction membrane 1101, and enters the collection dock 12. The cleaning solvent flows from the upper port 1201 through the outlet 1203, and sequentially enters the speed control valve 1501, the pump 1502, and the selection valve 1503. It then enters the inlet 1204 from the NC end of the selection valve 1503, flows out from the lower port 1202, passes through the dehydration device 13, and finally enters the collection bottle 14, achieving online dehydration. If the elution solvent needs to clean the sample bottle 5 during the elution process, the sample bottle cleaning process can be followed. However, the final eluent needs to pass through the NC end of the selection valve 1503 to be collected in the collection bottle 14.
[0048] The above description is illustrative only and not restrictive of the present invention. Those skilled in the art will understand that many modifications, variations or equivalents can be made without departing from the spirit and scope defined by the claims, and all such modifications, variations or equivalents will fall within the protection scope of the present invention.
Claims
1. A system flow path for solid phase extraction, characterized by: The rotary valve (1) has several solvent inlet ports (102), one solvent outlet port (103), and one waste liquid port (104) arranged around its circumference. The rotary valve (1) has a pump inlet port (101) arranged below it. One end of the pump inlet port (101) is connected to the syringe pump (3), and the other end of the pump inlet port (101) is connected to the common channel (105). The common channel (105) is also connected to one of the solvent inlet ports (102), the solvent outlet port (103), and the waste liquid port (104) through the rotation of the selection channel (106). The solvent inlet port (102) is connected to the solvent bottle (2), and the solvent outlet port (103) is connected to the sample loader (7). The gas path system (4) is connected to the pipeline between the rotary valve (1) and the sample loader (7). The sample loader (7) is provided with several channels. The sample loader (7) includes a valve core (8) and a valve body (9). The sample loader (7) controls the connection of the channels by rotating the valve core (8). A membrane adapter (11) is provided below the sample loader (7). An upper port (1201) is provided at the top of the collection dock (12), and the upper port (1201) is connected to the membrane adapter (11). A lower port (1202) is provided at the bottom of the collection dock (12), and the lower port (1202) is connected to the dewatering device (13) and the collection bottle (14). An outlet (1203) and an inlet (1204) are provided on the collection dock (12), and the outlet (1203) and the inlet (1204) are connected to the flow path switching system (15). A pressure balance port (1205) is also provided on the collection dock (12), and the pressure balance port (1205) is connected to the outside to balance the pressure inside the collection bottle (14). The top of the valve body (9) is connected to the sample bottle (5). The top of the valve body (9) is also provided with a spray needle (6) and placed inside the sample bottle (5). The bottom of the valve body (9) is also provided with a guide tube (907). The valve body (9) is provided with longitudinal channels, namely a main solvent channel (903), a spray channel (905) and a sample flow channel (906). The bottom end of the main solvent channel (903) is provided with a solvent interface (901). The pipeline between the solvent interface (901) and the solvent outlet port (103) is connected to the gas circuit system (4). The valve body (9) is also provided with transverse channels, namely an activation solvent channel (902) and a cleaning solvent channel (904). The main solvent channel (903) is connected to the activation solvent channel (902) and the cleaning solvent channel (904) respectively. The spray channel (905) is connected to the spray needle (6). The sample flow channel (906) is connected to the guide tube (907). The valve body (9) is provided with the valve core (8), and the valve core (8) is provided with the sample loading channel (801), the cleaning channel (802) and the activation channel (803). When the valve core (8) is rotated to the open position, the sample loading channel (801) is rotated to a position coaxial with the sample flow channel (906), and the spray channel (905), the cleaning channel (802), the cleaning solvent channel (904) and the main solvent channel (903) are connected. When the valve core (8) is rotated to the closed position, the sample loading channel (801) is rotated to a position not connected with the sample flow channel (906), and the main solvent channel (903), the activation solvent channel (902), the activation channel (803) and the sample flow channel (906) are connected.
2. The system flow path for solid phase extraction of claim 1, wherein: The gas system (4) includes an on / off valve (401), a pressure regulating valve (402) and a gas source (403). The pressure regulating valve (402) and the on / off valve (401) are sequentially installed at the top of the gas source (403) to regulate the gas pressure and open / close the gas pipeline.
3. The system flow path for solid phase extraction of claim 2, wherein: A liquid level sensor (10) is installed inside the membrane adapter (11) to monitor the liquid level. An extraction membrane (1101) is placed inside the membrane adapter (11), and a filter medium (1102) is added to the extraction membrane (1101).
4. The system flow path for solid phase extraction of claim 3, wherein: The flow path switching system (15) includes a speed control valve (1501), a liquid pump (1502), a selection valve (1503), a waste liquid selection valve (1504), an aqueous waste liquid tank (1505), and an organic waste liquid tank (1506). The C-end of the speed control valve (1501) is connected to the liquid outlet (1203), and the NC-end of the speed control valve (1501) is connected to the inlet of the liquid pump (1502). The outlet is connected to the C end of the selector valve (1503), the NC end of the selector valve (1503) is connected to the inlet (1204), the NO end of the selector valve (1503) is connected to the C end of the waste liquid selector valve (1504), the NO end of the waste liquid selector valve (1504) is connected to the water system waste liquid tank (1505), and the NC end of the waste liquid selector valve (1504) is connected to the organic system waste liquid tank (1506).
5. A method for applying a solid-phase extraction system flow path, implemented using the solid-phase extraction system flow path described in claim 4, characterized in that: When the system requires activation, rotate the selection channel (106) of the rotary valve (1) to one of the solvent inlet ports (102). The injection pump (3) draws the activation solvent from the solvent bottle (2). Then rotate the selection channel (106) to the solvent outlet port (103). The injection pump (3) pushes out the activation solvent. The activation solvent enters the main solvent channel (903) from the solvent interface (901). At this time, the valve core (8) is in the closed state. The sample loading channel (801) and the sample flow channel (906) are not connected. The spray channel (905) and the cleaning solvent channel (904) are closed by the valve core (8). The activation solvent can only flow into the activation solvent channel (902) and the activation channel. (803), then flows into the lower half of the sample flow channel (906), and finally flows through the guide tube (907) into the membrane adapter (11) to activate the extraction membrane (1101). The activation solvent passes through the filter medium (1102) and the extraction membrane (1101) into the collection dock (12). The activation solvent flows from the upper port (1201) through the outlet (1203) and enters the speed control valve (1501), the liquid pump (1502), and the selection valve (1503) in sequence. It flows out from the NO end of the selection valve (1503) and finally enters the water system waste liquid tank (1505) or the organic system waste liquid tank (1506) through the waste liquid selection valve (1504) according to the waste liquid type, so as to realize the waste liquid classification and collection. When the system requires rinsing, the process is the same as the activation process described above, and a solvent is selected to clean the extraction membrane (1101); When the system requires sample loading, the valve core (8) is in the open state, the sample loading channel (801) and the sample flow channel (906) are connected, and the sample flows out from the sample bottle (5) into the membrane adapter (11). At this time, the rotary valve (1) is in the closed position. Although the solvent interface (901), the main solvent channel (903) and the spray channel (905) are connected, the sample will not flow away from the spray channel (905) and be lost. The liquid remaining in the pipeline is blown back into the sample bottle (5) through the gas system (4). The liquid level of the membrane adapter (11) is monitored by the liquid level sensor (10) and controlled. The valve core (8) is opened and closed to prevent the sample from overflowing from the membrane adapter (11). Dirt particles in the sample are intercepted by the filter medium (1102), and the effective substances in the sample are adsorbed by the extraction membrane (1101). The waste liquid enters the collection dock (12). The waste liquid flows from the upper port (1201) through the outlet (1203) and enters the speed control valve (1501), the pump (1502), and the selection valve (1503) in sequence. It flows out from the NO end of the selection valve (1503) and finally enters the water system waste liquid tank (1505) through the NO end of the waste liquid selection valve (1504) according to the waste liquid type. When the system requires cleaning the sample vial, rotate the selection channel (106) of the rotary valve (1) to one of the solvent inlet ports (102). The injection pump (3) draws the cleaning solvent from the solvent vial (2). Then rotate the selection channel (106) to the solvent outlet port (103). The valve core (8) is in the open state. Then open the gas path system (4). The cleaning solvent and gas enter together from the solvent interface (901), flow sequentially through the main solvent channel (903), the cleaning solvent channel (904), the cleaning channel (802), and finally enter the spray needle (6) from the spray channel (905) to clean the sample vial (5). After the cleaning solvent is sprayed... After the sample bottle (5) is placed, the cleaning solvent enters the membrane adapter (11) through the sample flow channel (906) and the guide tube (907). The cleaning solvent passes through the filter medium (1102) and the extraction membrane (1101) and enters the collection dock (12). The cleaning solvent flows from the upper port (1201) through the liquid outlet (1203) and sequentially enters the speed control valve (1501), the liquid pump (1502), and the selection valve (1503). It flows out from the NO end of the selection valve (1503) and finally enters the water system waste liquid tank (1505) or the organic system waste liquid tank (1506) through the waste liquid selection valve (1504) according to the waste liquid type, so as to realize the classified collection of waste liquid. When the system requires elution, the selection channel (106) of the rotary valve (1) is rotated to one of the solvent inlet ports (102), and the injection pump (3) draws the elution solvent from the solvent bottle (2). Then, the selection channel (106) is rotated to the solvent outlet port (103), and the injection pump (3) pushes out the elution solvent. The valve core (8) is closed, and the elution solvent enters the main solvent channel (903) from the solvent interface (901). The elution solvent can only flow into the activation solvent channel (902) and the activation channel (803), and then into the lower half of the sample flow channel (906). Finally, it flows through the guide tube (907) to the membrane adapter (11) to elute the substances adsorbed on the extraction membrane (1101). The elution solvent passes through the filter medium (1102) and the extraction membrane (1101) and enters the collection dock (12). The cleaning solvent flows from the upper port (1201) through the liquid outlet (1203) and sequentially enters the speed control valve (1501), the liquid pump (1502), and the selection valve (1503). It enters the liquid inlet (1204) from the NC end of the selection valve (1503), flows out from the lower port (1202), flows through the water removal device (13), and finally enters the collection bottle (14) to achieve online water removal. If the elution solvent needs to clean the sample bottle (5) during the elution process, the sample bottle cleaning process can be followed. However, the final eluent needs to pass through the NC end of the selection valve (1503) and be collected in the collection bottle (14).
Citation Information
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