An on-line sampling dilution device

Abstract

An online sampling and dilution device includes a reaction solution (1), an injection pump (2), a selection valve (3), a first three-way solenoid valve (4), a second three-way solenoid valve (5), a sample needle (6), a diluent (7), a sample vial (8), an air filter (9), a waste liquid tank (10), and a controller (11). The reaction solution (1) is connected to the selection valve (3), the injection pump (2) is connected to the selection valve (3), the first three-way solenoid valve (4) is connected to the selection valve (3), the sample needle (6), and the second three-way solenoid valve (5), the second three-way solenoid valve (5) is connected to the first three-way solenoid valve (4), the reaction solution (1), and the waste liquid tank (10), the sample needle (6) is connected to the first three-way solenoid valve (4), the diluent (7) is connected to the selection valve (3), and the air filter (9) is connected to the selection valve (3). The online sampling and dilution device of the present invention has the advantages of low rinsing volume, accurate sampling concentration, no sample loss, and precise sampling and dilution.

Description

Technical Field

[0001] This invention relates to an online sampling and dilution device, belonging to the fields of medicine, biology, and chemical engineering, and in particular to an online sampling and dilution device that can perform timed sampling and precise dilution of chemical reactions or fermentation processes. Background Technology

[0002] Chemical synthesis reactions, especially organic synthesis reactions, are generally quite complex, and many factors affect the reaction. Therefore, different devices are needed for different reactions depending on the reaction conditions, such as reaction temperature, reaction time, material addition method and sequence, and whether the reaction needs to be stirred.

[0003] Fermentation refers to the process by which microorganisms, under aerobic or anaerobic conditions, produce the microbial cells themselves, or their direct or secondary metabolites. Fermentation is one of the earliest biochemical reactions humans encountered and is now widely used in the food, biological, and chemical industries.

[0004] In chemical synthesis reactions or fermentation processes, it is often necessary to continuously sample and monitor the reaction or fermentation process. The samples typically need to be accurately diluted before being injected into a high-performance liquid chromatograph (HPLC) for analysis. Current solutions usually involve manually sampling into sample vials, followed by quantitative dilution, a cumbersome process. The sample volume is often larger than the actual requirement to prevent insufficient sampling, which wastes sample in small exploratory reactions (e.g., a few milliliters of reaction volume) and affects the reaction yield. Sampling also requires opening the reaction flask, which can negatively impact anaerobic reactions (nitrogen protection) and is detrimental to the reaction. Summary of the Invention

[0005] To address the aforementioned shortcomings of existing processing methods, the present invention aims to provide an online sampling and dilution device that can perform precise sampling and dilution at user-defined sampling time points. The entire process is carried out in a sealed environment, minimizing the impact on the reaction, ensuring rapid and thorough rinsing, accurate sampling concentration, and quantitative dilution of the sample during sampling, allowing users to directly perform testing.

[0006] To achieve the above objectives, the present invention adopts the following technical solution: An online sampling and dilution device includes a reaction solution (1), an injection pump (2), a selection valve (3), a first three-way solenoid valve (4), a second three-way solenoid valve (5), a sample needle (6), a diluent (7), a sample vial (8), an air filter (9), a waste liquid tank (10), and a controller (11). The reaction solution (1) is connected to the selection valve (3), the injection pump (2) is connected to the selection valve (3), the first three-way solenoid valve (4) is connected to the selection valve (3), the sample needle (6), and the second three-way solenoid valve (5), the second three-way solenoid valve (5) is connected to the first three-way solenoid valve (4), the reaction solution (1), and the waste liquid tank (10), the sample needle (6) is connected to the first three-way solenoid valve (4), the diluent (7) is connected to the selection valve (3), the air filter (9) is connected to the selection valve (3), and the controller (11) controls each component to perform the sampling and dilution process.

[0007] Preferably, the online sampling and dilution device further includes a reagent addition device (12), which is connected to the selection valve (3) and can add a set volume of reagent to the reaction solution at a user-set time.

[0008] Preferably, the sample vial (8) is equipped with a sealing cap, and the sample needle (6) can be inserted into the sample vial (8) to perform sample sorting, so as to avoid changes in sample concentration caused by solvent evaporation during long-term storage.

[0009] Preferably, the sample bottle (8) is placed on a refrigerated tray to preserve the sample at low temperature, thereby improving the sample stability. Beneficial effects

[0010] (1) The entire process is carried out online and in a sealed environment, which has no effect on the reaction.

[0011] (2) The rinsing is quick and thorough to ensure the accuracy of the sample concentration.

[0012] (3) The sampling is accurate. The rinsing, injection pump head and tail cut-off and the reaction liquid in the pipeline are also returned to the reaction liquid to continue to participate in the reaction, which has little impact on the reaction yield.

[0013] (4) Sampling and dilution are completed simultaneously, and the dilution is accurate. Users can directly use the sample for HPLC injection. Attached Figure Description

[0014] Figure 1 This is a schematic diagram of Embodiment 1 of an online sampling and dilution device of the present invention. In the diagram: 1. Reaction flask, 2. Injection pump, 3. Selector valve, 4. First three-way solenoid valve, 5. Second three-way solenoid valve, 6. Sample needle, 7. Diluent, 8. Sample vial, 9. Air filter, 10. Waste container, 11. Controller, 12. Reagent addition. Detailed Implementation

[0015] The preferred embodiments of the present invention will now be described in detail with reference to the accompanying drawings. Example

[0016] like Figure 1 As shown, an online sampling and dilution device includes a reaction flask, a syringe pump, a selection valve, a first three-way solenoid valve, a second three-way solenoid valve, a sample needle, a diluent, a sample vial, an air filter, a waste liquid tank, and a controller.

[0017] The operating procedure of the online sampling and dilution device is as follows: 1. Rinsing: (a) Sample extraction: Select valve (3) to pass reaction solution (1), and use injection pump (2) to extract a certain volume of reaction solution; (b) Sample ejection: Select valve (3) opens the first three-way solenoid valve (4), the first three-way solenoid valve (4) opens the second three-way solenoid valve (5), the second three-way solenoid valve (5) opens the reaction liquid (1), and the injection pump (2) ejects the reaction liquid; (c) Repeat this process multiple times to perform the rinsing.

[0018] 2. Sampling: (a) Sample extraction: Select valve (3) to pass reaction solution (1), and use injection pump (2) to extract a certain volume of reaction solution; (b) Pre-push sample: Select valve (3) opens the first three-way solenoid valve (4), the first three-way solenoid valve (4) opens the second three-way solenoid valve (5), the second three-way solenoid valve (5) opens the reaction liquid (1), and the injection pump (2) pushes out a small amount of reaction liquid to remove air bubbles; (c) Sample discharge: Select valve (3) opens the first three-way solenoid valve (4), the first three-way solenoid valve (4) opens the sample needle (6), the sample needle (6) is inserted into the sample bottle (8), the syringe pump (2) pushes out the specified volume, and the sample discharge is performed; (d) Push back the remaining sample: Select valve (3) opens the first three-way solenoid valve (4), the first three-way solenoid valve (4) opens the second three-way solenoid valve (5), the second three-way solenoid valve (5) opens the reaction liquid (1), the injection pump (2) is reset, and the remaining sample is pushed back; 3. Purge: (a) Air extraction: Select valve (3) through air filter (9), and injection pump (3) extract a certain volume of air; (b) Purge the sample needle: Select valve (3) opens the first three-way solenoid valve (4), the first three-way solenoid valve (4) opens the sample needle (6), and the syringe pump pushes out 0.5 mL to basically drain the liquid from the sample needle; (c) Emptying the sample needle: The syringe pump (2) performs small aspiration and large push (simulating the operation of a pipette), such as drawing 0.2 mL and pushing out 0.4 mL, repeating this until the needle is reset, so as to empty the liquid in the sample needle; 4. Emptying: (a) Air extraction: Select valve (3) through air filter (9), and injection pump (3) extract a certain volume of air; (b) Emptying the pipeline: Select valve (3) connects to the first three-way solenoid valve (4), the first three-way solenoid valve (4) connects to the second three-way solenoid valve (5), the second three-way solenoid valve (5) connects to the reaction liquid (1), the injection pump (2) is reset, and the pipeline is emptied; 5. Dilution: (a) Extracting diluent: Select valve (2) to pass diluent (7), and syringe pump (3) to extract a certain volume of diluent; (b) Pre-push diluent: Select valve (3) opens the first three-way solenoid valve (4), the first three-way solenoid valve (4) opens the second three-way solenoid valve (5), the second three-way solenoid valve (5) opens the waste liquid tank (10), and the injection pump (2) pushes out a small amount of diluent to remove air bubbles; (c) Discharge of diluent: Select valve (3) opens the first three-way solenoid valve (4), the first three-way solenoid valve (4) opens the sample needle (6), the sample needle (6) is inserted into the sample vial (8), and the syringe pump (2) pushes out the specified volume to discharge the diluent; (d) Discharge the remaining diluent: Select valve (3) opens the first three-way solenoid valve (4), the first three-way solenoid valve (4) opens the second three-way solenoid valve (5), the second three-way solenoid valve (5) opens the waste liquid tank (19), the injection pump (2) is reset, and the remaining diluent is discharged; (c) This process can be repeated multiple times to perform the dilution; (d) Air extraction: Select valve (3) through air filter (9), and injection pump (3) extract a certain volume of air; (e) Purge the sample needle: Select valve (3) opens the first three-way solenoid valve (4), the first three-way solenoid valve (4) opens the sample needle (6), and the syringe pump pushes out 0.5 mL to basically drain the liquid from the sample needle; (f) Emptying the sample needle: The syringe pump (2) performs small aspiration and large push (simulating the operation of a pipette), such as drawing 0.2 mL and pushing out 0.4 mL, repeating this until it is reset, so as to empty the liquid in the sample needle; Using purified water as the medium, a sampling dilution procedure was performed (sample volume 0.5 mL, dilution volume 0.5 mL) to verify the accuracy of the sampling dilution. The results are as follows: 1 2.8224 3.8176 0.9952 2 2.9055 3.9073 1.0018 3 2.8372 3.8422 1.0050 4 2.8218 3.8223 1.0005 5 2.9106 3.9131 1.0025 6 2.8893 3.9012 1.0119 average value 1.0028 RSD 0.55% The results showed that the sampling and dilution accuracy was good.

Claims

1. An online sampling and dilution device, characterized in that: The device includes a reaction solution (1), an injection pump (2), a selector valve (3), a first three-way solenoid valve (4), a second three-way solenoid valve (5), a sample needle (6), a diluent (7), a sample vial (8), an air filter (9), a waste container (10), and a controller (11). The reaction solution (1) is connected to the selector valve (3), the injection pump (2) is connected to the selector valve (3), the first three-way solenoid valve (4) is connected to the selector valve (3), the sample needle (6), and the second three-way solenoid valve (5), the second three-way solenoid valve (5) is connected to the first three-way solenoid valve (4), the reaction solution (1), and the waste container (10), the sample needle (6) is connected to the first three-way solenoid valve (4), the diluent (7) is connected to the selector valve (3), and the air filter (9) is connected to the selector valve (3).

2. The online sampling and dilution device according to claim 1, characterized in that: The online sampling and dilution device also includes a reagent addition device (12), which is connected to the selection valve (3) and can add a set volume of reagent to the reaction solution at a user-defined time point.

3. An online sampling and dilution device according to claim 1 or 2, characterized in that: The sample vial (8) is equipped with a sealing cap, and the sample needle (6) can be inserted into the sample to perform sample removal, so as to avoid changes in sample concentration caused by solvent evaporation during long-term storage.

4. An online sampling and dilution device according to claim 1 or 2, characterized in that: The sample vial (8) is placed on a refrigerated tray to preserve the sample at low temperatures, thereby improving the sample stability.

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