Sample injection device, control method for sample injection device, and liquid monitoring and analyzing instrument
By combining a gas-liquid actuator, a multi-way valve, and a three-way valve, along with a fixed-length quantitative tube and a carrier gas/pure water control method, the problems of inaccurate quantification, complex structure, and difficult cleaning of existing sample injection devices are solved. This achieves precise control of sample injection volume, simplifies the device, and reduces costs.
Patent Information
- Authority / Receiving Office
- WO · WO
- Patent Type
- Applications
- Current Assignee / Owner
- SHIMADZU (CHINA) CO LTD
- Filing Date
- 2025-10-24
- Publication Date
- 2026-07-02
Smart Images

Figure CN2025129831_02072026_PF_FP_ABST
Abstract
Description
Sampling device, control method of sampling device, liquid monitoring and analysis instrument Technical Field
[0001] This invention relates to the field of analytical technology, and more specifically to a sample injection device, a control method for the sample injection device, a liquid monitoring analyzer having the sample injection device, and a liquid monitoring analyzer using the control method for the sample injection device. Background Technology
[0002] As a front-end device of chemical analysis instruments, the sample introduction device is widely used in many fields such as environmental monitoring, health and medicine, and inspection and quarantine. Among them, the sample introduction device needs to accurately quantify the introduced sample.
[0003] Existing sample quantification methods in sample introduction devices, such as the one disclosed in Chinese patent document CN118533601A, include a digestion measurement module, a peristaltic pump, a liquid supply device, a quantitative tube, and multiple liquid level sensors. The peristaltic pump is connected to a first valve body; the liquid supply device forms multiple liquid storage chambers; one end of the quantitative tube is connected to a second valve body, and the other end is connected to a common interface of a rotary valve. Multiple selection interfaces of the rotary valve correspond one-to-one with and are connected to the multiple liquid storage chambers. The quantitative tube has multiple liquid level detection positions; the multiple liquid level sensors correspond one-to-one with the multiple liquid level detection positions, and the liquid level sensors are used to detect the liquid presence at the corresponding liquid level detection position, thereby detecting the sample volume introduced into the quantitative tube.
[0004] The existing sample introduction devices described above require a peristaltic pump to deliver the sample and necessitate multiple liquid level detection points and corresponding liquid level sensors in the metering tube. However, the flow rate of the liquid delivered by the peristaltic pump fluctuates, affecting the accuracy of the quantification. Furthermore, the metering tube must be transparent to accommodate the liquid level sensors, resulting in a complex device with numerous electrical components and high production and maintenance costs. Additionally, the metering tubes in these existing technologies require the injection and extraction of pure water into the detection cell for cleaning, which can hinder thorough cleaning.
[0005] Therefore, how to achieve a sample introduction device that is accurate in quantification, simple in structure, low in cost, and easy to clean is a current challenge. Summary of the Invention
[0006] To address the above problems, this invention provides a sample introduction device and a water quality analyzer incorporating the device. By implementing the control method for the sample introduction device provided by this invention on the aforementioned equipment, the sample volume entering the analyzer can be made more precise, and the stability of the sample volume can be ensured even with multiple injections. Simultaneously, the structure of existing sample introduction devices is simplified, further reducing the installation and maintenance costs. Furthermore, it also allows for more thorough cleaning of the quantitative tube.
[0007] The first aspect of this invention provides a sample introduction device, comprising: a gas-liquid actuator, a multi-way valve, a quantitative tube, a three-way valve, and an analytical tube. The multi-way valve includes an actuator valve port connected to the gas-liquid actuator, a sample end valve port connected to the sample end, a carrier gas end valve port connected to the carrier gas end, and a quantitative tube valve port; one end of the quantitative tube is connected to the quantitative tube valve port; the three-way valve includes a first port, a second port, and a third port, the first port being connected to the other end of the quantitative tube, and the third port being connected to the outside environment; the analytical tube is connected to the second port of the three-way valve.
[0008] In the optional technical solution, one end of the injection block is connected to the second port of the three-way valve, and the other end is connected to the analysis tube.
[0009] In the optional technical solutions, the internal volume of the quantitative tube is the specified capacity.
[0010] In the alternative technical solutions, the gas-liquid actuator can be either a syringe or a plunger pump.
[0011] In optional technical solutions, the volume of gas or liquid that can be drawn by the syringe or plunger pump is at least greater than the internal volume of the metering tube.
[0012] In optional technical solutions, the multi-way valve also includes a pure water end valve port, which is connected to an external pure water source.
[0013] A second aspect of the present invention provides a control method for a sample injection device, used in the aforementioned sample injection device, the control method specifically including the following steps:
[0014] The sample conduction step controls the connection between the driver valve port and the sample end valve port of the multi-way valve.
[0015] In the sample extraction step, the gas-liquid actuator is controlled to extract a first predetermined amount of sample into the gas-liquid actuator through the sample end valve port.
[0016] The metering tube conduction procedure controls the connection between the metering tube valve and the gas-liquid actuator.
[0017] The first mode of the three-way valve is activated by controlling the activation of the first and third ports of the three-way valve.
[0018] In the sample injection metering tube step, the gas-liquid actuator is controlled to push a first predetermined amount of sample into the metering tube.
[0019] The carrier gas conduction step controls the connection between the actuator valve port and the carrier gas end valve port of the multi-way valve.
[0020] Carrier gas extraction step: Control the gas-liquid actuator to extract a first predetermined amount of carrier gas;
[0021] The second mode of the three-way valve is activated by controlling the activation of the first and second ports of the three-way valve.
[0022] In the carrier gas injection metering tube step, the gas-liquid actuator is controlled to push a first predetermined amount of carrier gas to push the sample in the metering tube.
[0023] In the optional technical solution, the volume of the first predetermined sample is greater than the internal volume of the quantitative tube.
[0024] In the optional technical solution, the volume of the first predetermined amount of carrier gas is greater than the internal volume of the metering tube.
[0025] Among the optional technical solutions, the control method for the sample introduction device also includes:
[0026] Cleaning preparation steps: Control the gas-liquid actuator to draw a first predetermined amount of pure water into the gas-liquid actuator through the pure water end valve port.
[0027] The metering tube conduction procedure controls the connection between the metering tube valve and the gas-liquid actuator.
[0028] The metering tube cleaning step involves controlling the gas-liquid actuator to push a predetermined amount of pure water into the metering tube.
[0029] In the optional technical solution, the volume of the first predetermined amount of pure water is greater than the internal volume of the metering tube.
[0030] A third aspect of the present invention provides a liquid monitoring and analysis instrument, including the above-described sample introduction device.
[0031] In an optional technical solution, the liquid monitoring analyzer performs the control method of the above-mentioned sample introduction device.
[0032] This invention, by specifically placing a quantitative tube of fixed length between a multi-way valve and a three-way valve within the sample introduction device, uses the internal volume of the quantitative tube as the sample injection volume. This ensures precise and controllable sample injection volume and maintains consistency in the amount of sample entering the analysis device during multiple injections. Simultaneously, the multi-way and three-way valves allow for various connections and switching between multiple gas or liquid sampling ports, the analysis tube, and the external environment. This enables the sample introduction device to quickly switch between injection and cleaning modes, allowing for rapid sequential quantitative analysis of multiple samples. Furthermore, it avoids interference between different samples during the injection and analysis process, ensuring the stability and accuracy of the analytical results. Attached Figure Description
[0033] Figure 1 is a schematic diagram of a sample introduction device provided in an embodiment of the present invention.
[0034] Figure 2 is a schematic diagram of another sample introduction device provided in an embodiment of the present invention.
[0035] Figure 3 is a flowchart of a control method for a sample injection device provided by an embodiment of the present invention.
[0036] Figure 4 is a flowchart of another control method for a sample introduction device provided by an embodiment of the present invention.
[0037] Reference numerals: 100-Injection device, 1-Gas-liquid actuator (syringe), 11-Empty syringe barrel, 12-Piston, 13-Needle, 14-Tube, 2-Multi-port valve, 21-Actuator valve port, 22-Sample end valve port, 23-Carrier gas end valve port, 24-Pure water end valve port, 25-Quantitative tube valve port, 3-Quantitative tube, 4-Three-way valve, 41-First port, 42-Second port, 43-Third port, 5-Injection block, 6-Analytical tube, 7-Sample end, 8-Carrier gas end, 9-Pure water source, 10-Waste gas recovery device, 11-Waste liquid recovery device. Detailed Implementation
[0038] The technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.
[0039] <First Implementation Method>
[0040] Figure 1 is a schematic diagram of the structure of a sample injection device 100 provided by the present invention. As shown in Figure 1, the sample injection device 100 includes: a gas-liquid actuator 1, a multi-way valve 2, a quantitative tube 3, a three-way valve 4, and an analysis tube 6.
[0041] Referring to Figure 1, in this embodiment, the multi-way valve 2 includes a driver valve port 21, a sample end valve port 22, a carrier gas end valve port 23, and a metering tube valve port 25. The sample end valve port 22 is connected to the sample end 7 where the liquid sample to be analyzed is stored, and the carrier gas end valve port 23 is connected to the carrier gas end 8 where the carrier gas is stored. By switching the valve ports of the multi-way valve 2, the metering tube valve port 25 can be connected to any one of the valve ports within the multi-way valve 2.
[0042] In this embodiment, the gas-liquid actuator 1 can be a syringe, which includes a syringe barrel 11, a piston 12, a needle 13, and a conduit 14. By applying a pulling or pushing force to the piston 12 of the syringe, gas or liquid is drawn into the syringe barrel 11 or pushed out of the syringe barrel 11. The external force applied to the piston 12 can be provided manually or by a mechanical device (not shown in the figure). The syringe barrel 11 is connected to the actuator port 21 of the multi-way valve 2 through the needle 13 and the conduit 14. The conduit 14 can be a corrosion-resistant rubber hose or a metal hose, or other materials; no specific limitation is made here. In other embodiments of the present invention, the conduit 14 can be omitted, and the syringe needle 13 can be directly connected to the actuator port 21 of the multi-way valve 2.
[0043] Referring to Figure 1, the syringe barrel 11 is preferably made of a transparent material and has graduated lines on its surface. By observing the graduated lines corresponding to the end of the syringe piston 12 inside the syringe barrel 11 or by detecting the stroke of the syringe piston 12, the volume of gas or liquid inside the syringe barrel 11 can be accurately determined, thereby allowing for a simple and quick assessment of the actual liquid or gas intake within the syringe (gas-liquid actuator 1). In other embodiments of the present invention, the gas-liquid actuator 1 may also be a plunger pump, which is not limited here.
[0044] As shown in Figure 1, in this embodiment, the three-way valve 4 has a first port 41, a second port 42, and a third port 43. By adjusting the valve port switch of the three-way valve 4, any two of the ports can be connected. One end of the metering tube 3 is connected to the metering tube valve port 25 of the multi-way valve 2, and the other end is connected to the first port 41 of the three-way valve 4.
[0045] Referring to Figure 1, the analysis tube 6 in the sample introduction device 100 is used for the detection and analysis of the sample liquid. The second port 42 of the three-way valve 4 is connected to the sample inlet (not shown in the figure) of the analysis tube 6. The third port 43 of the three-way valve 4 is connected to both the waste gas recovery device 10 and the waste liquid recovery device 11.
[0046] Preferably, in this embodiment, the sample injection device 100 is further provided with a sample injection block 5, one end of which is connected to the second port 42 of the three-way valve 4, and the other end is connected to the analysis tube 6. It can be used to pre-treat the sample solution liquid entering the analysis tube 6 so that the sample meets the analysis conditions.
[0047] The connection relationships of the various components of the sample injection device 100 in this embodiment have been explained above. The operation of the sample injection device 100 will be explained below.
[0048] <Extracting Sample Liquid>
[0049] The sample end 7 is used to store the sample liquid to be analyzed. By connecting the sample end 7 to the sample end valve port 22 and switching the valve port of the multi-way valve 2 to connect the sample end valve port 22 to the driver valve port 21, the syringe piston 12 can be pulled to draw the sample liquid into the syringe empty cylinder 11 and store it inside the syringe empty cylinder 11. In other embodiments, the sample injection device 100 may also be provided with multiple sample ends 7, and the multi-way valve 2 may be provided with multiple sample end valve ports 22. By sequentially switching the valve port of the multi-way valve 2 to each sample end valve port 22, multiple samples can be rapidly injected for analysis. The specific number of sample ends 7 and sample end valve ports 22 is not limited here.
[0050] <Injecting sample liquid>
[0051] After the sample liquid is drawn into the syringe empty cylinder 11, the valve port of the multi-way valve 2 is switched so that the driver valve port 21 is connected to the metering tube valve port 25, and the three-way valve 4 is switched so that the first port 41 is connected to the third port 43.
[0052] In the above state, push the syringe piston 12 so that the sample solution accumulated in the syringe empty cylinder 11 is injected into the quantitative tube 3 through the quantitative tube valve port 25, until a portion of the sample liquid flows into the waste liquid recovery device 11 through the first port 41 and the third port 43.
[0053] As shown in Figure 1, in this embodiment, the syringe (gas-liquid actuator 1) is preferably configured with the syringe barrel 11 perpendicular to the ground and the needle 13 pointing upwards. This configuration allows any residual gas in the syringe barrel 11 and the sample injection device 100 to first pass through the metering tube 3 before being discharged to the outside or waste gas recovery device 10 from the third port 43 when the syringe (gas-liquid actuator 1) and the tubing are completely emptied. After the residual gas in the syringe (gas-liquid actuator 1) and the tubing is completely emptied, the piston 12 continues to be pushed, allowing the sample liquid in the syringe barrel 11 to fully enter the metering tube 3. When the sample liquid is detected flowing through the third port 43 to the waste liquid recovery device 11, it indicates that the metering tube 3 is now full of sample liquid.
[0054] As long as the metering tube 3 itself is not replaced, the internal volume of the metering tube 3 located between the first port 41 of the three-way valve 4 and the metering tube valve port 25 of the multi-way valve 2 is preset and fixed. Therefore, the amount of sample liquid filling the internal volume of the metering tube 3 is the internal volume of the metering tube 3, thereby enabling accurate quantification of the sample liquid.
[0055] Of course, in other embodiments of the present invention, the syringe needle 13 may also be set at an angle upward, as long as it is ensured that when the residual gas in the syringe empty cylinder 11 is emptied, there is still enough sample liquid to fill the quantitative tube 3.
[0056] <Carrier Gas Extraction>
[0057] After injecting the sample liquid and filling the metering tube 3, switch the valve port of the multi-port valve 2 so that the driver valve port 21 is connected to the carrier gas end valve port 23. Then, pull the syringe piston 12 again so that the carrier gas stored in the carrier gas end 8 can be drawn into the syringe empty cylinder 11 and stored inside the syringe empty cylinder 11.
[0058] The carrier gas end 8 is used to store the carrier gas that propels the liquid in the pipeline of the sample injection device 100. The carrier gas can be an inert gas such as nitrogen or argon to avoid the carrier gas reacting with the sample liquid and thus affecting the analysis results.
[0059] <Carrier Gas Injection>
[0060] After the carrier gas is drawn into the empty syringe barrel 11, the valve port of the multi-way valve 2 is switched so that the driver valve port 21 is connected to the metering tube valve port 25, and the three-way valve 4 is switched so that the first port 41 is connected to the second port 42.
[0061] In the above-mentioned connected state, pushing the syringe piston 12 causes the carrier gas accumulated in the syringe barrel 11 to be injected into the quantitative tube 3 through the quantitative tube valve port 25. At this time, the sample liquid quantitatively accumulated inside the quantitative tube 3 is propelled by the carrier gas and flows into the analysis tube 6 through the first port 41 and the second port 42. This enables the precise quantitative analysis of the sample liquid.
[0062] Preferably, the volume of gas or liquid that the syringe (gas-liquid actuator 1) can draw, i.e., the volume of the syringe empty cylinder 11 in this embodiment, is at least greater than the internal volume of the metering tube 3. Because when the volume of the syringe empty cylinder 11 is greater than the internal volume of the metering tube 3, the syringe empty cylinder 11 can draw the stored sample liquid or carrier gas, completely filling and overflowing the inside of the metering tube 3, thereby ensuring that the sample liquid fills the internal volume of the metering tube 3, so as to achieve accurate quantification of the sample liquid.
[0063] In this embodiment, the length of the quantitative tube 3 is set to a fixed value (i.e., the length of the quantitative tube 3 between the quantitative tube valve port 25 and the first port 41), so that the internal volume of the quantitative tube 3 is a predetermined capacity, which is the injection volume of the liquid sample to be analyzed. This embodiment uses a quantitative tube 3 of fixed length. When the quantitative tube 3 is full of liquid, by adjusting the valve ports of the multi-way valve 2 and the three-way valve 4, the carrier gas pre-stored in the syringe empty cylinder 11 is used to push all the liquid sample in the quantitative tube 3 into the analysis tube 6. This embodiment ensures that the injection volume of the liquid sample into the analysis tube 6 is precise and fixed, thereby guaranteeing the stability and accuracy of the analysis results. Simultaneously, the quantitative tube 3 also functions as a transporter of gas or other liquids. The material of the quantitative tube 3 can be a corrosion-resistant metal or other materials, and is not limited here. The quantitative tube 3 shown in Figure 1 is a straight type. In other embodiments, the quantitative tube 3 can also be arranged in a ring shape according to the design length of the quantitative tube 3 and the specific usage environment, and is not limited here.
[0064] As described above, the sample injection device 100 provided according to this embodiment achieves accurate quantification of sample solution with an extremely simple structure without the need for electrical components such as liquid level detectors. The structure is simple and easy to operate and maintain.
[0065] <Second Implementation Method>
[0066] Figure 2 is a schematic diagram of another sample injection device 100 provided in the second embodiment of the present invention. The difference between the second embodiment and the first embodiment is that in the sample injection device 100 of the second embodiment, the multi-way valve 2 further has a pure water end valve port 24, which is connected to a pure water source 9 storing pure water.
[0067] In the second embodiment, the same structure as in the first embodiment is described using the same symbols, and will not be repeated here.
[0068] As shown in Figure 2, the pure water source 9 is used to store pure water for rinsing the pipeline of the sample injection device 100. The pure water is preferably deionized water to avoid introducing other impurities during pipeline rinsing, which could affect the sample analysis results. By connecting the pure water source 9 to the pure water end valve port 24 and switching the multi-way valve 2 port to connect the pure water end valve port 24 to the actuator valve port 21, pulling the syringe piston 12 allows the pure water in the pure water source 9 to be drawn into the syringe empty cylinder 11. Preferably, in this embodiment, the amount of pure water drawn into the gas-liquid actuator 1 (i.e., the syringe empty cylinder 11) is at least greater than the internal volume of the metering tube 3. Because when the amount of pure water drawn into the syringe empty cylinder 11 is greater than the internal volume of the metering tube 3, pushing the pure water in the syringe empty cylinder 11 into the metering tube 3 allows the metering tube 3 to be completely filled with pure water and overflow, thereby ensuring the rinsing effect of the metering tube 3.
[0069] The rinsing action of the sample introduction device 100 will be explained below.
[0070] <Quantitative tube flushing>
[0071] After pure water is drawn into the syringe barrel 11, the multi-way valve 2 is switched to connect the actuator valve 21 with the metering tube valve 25. Then, the three-way valve 4 is switched to connect the first port 41 with the third port 43. The syringe piston 12 is then pushed, causing the pre-drawn pure water in the syringe barrel 11 to flow through the multi-way valve 2 into the metering tube 3, and finally from the third port 43 to the waste liquid recovery device 11. During this process, residual gas in the sample injection device 100 pipeline can also be discharged through the third port 43 to the externally installed waste gas recovery device 10 for recovery. In this embodiment, when pure water flows out of the third port 43, it means that the inner surface of the metering tube 3 has been completely rinsed with pure water. To ensure the cleaning effect of the pipeline, the amount of pure water drawn into the syringe empty barrel 11 can be appropriately increased, thereby extending the rinsing time of the pipeline. Alternatively, after rinsing the metering tube 3 with pure water once, the valve port of the multi-way valve 2 can be switched again to connect the pure water end valve port 24 with the driver valve port 21, and the syringe piston 12 can be pulled to draw pure water into the syringe empty barrel 11, rinsing the metering tube 3 with pure water again. The rinsing process of the metering tube 3 can be repeated in this way.
[0072] <Analytical tube flushing>
[0073] After the rinsing process of the quantitative tube 3 is completed, the analytical tube 6 is rinsed with pure water. Specifically, the actuator valve port 21 is connected to the pure water end valve port 24, and the valve port of the three-way valve 4 is switched so that the first port 41 is connected to the second port 42. In the above state, the syringe piston 12 is pulled to draw pure water from the pure water end valve port 24 into the syringe empty barrel 11. Then, the valve port of the multi-way valve 2 is switched, and the syringe piston 12 is pushed so that the pure water accumulated in the syringe empty barrel 11 is injected into the quantitative tube 3 through the quantitative tube valve port 25 until the pure water flows into the sample block 5 and the analytical tube 6 in sequence through the first port 41 and the second port 42, and finally flows out from the discharge port of the analytical tube 6 (not shown in the figure), which means that the rinsing of the sample block 5 and the analytical tube 6 is completed.
[0074] To ensure the cleanliness of the analysis tube 6, the same method as rinsing the quantitative tube 3 can be used, by repeatedly drawing pure water from the pure water source 9 into the gas-liquid actuator 1 to repeat the rinsing process of the analysis tube 6.
[0075] Of course, if there is still enough pure water in the gas-liquid actuator 1 (i.e., syringe empty cylinder 11) after rinsing the quantitative tube 3, the actuator valve port 21 and the quantitative tube valve port 25 can be kept connected. Only the three-way valve 4 can be switched so that the first port 41 and the second port 42 are connected before rinsing the analysis tube 6.
[0076] <Third Implementation Method>
[0077] The present invention also provides a control method for a sample injection device 100, used in the sample injection device 100 provided in the above embodiments. Referring to FIG3, the steps of the control method include: sample conduction step S1, sample extraction step S2, quantitative tube conduction step S3, three-way valve first mode conduction step S4, sample injection into quantitative tube step S5, carrier gas conduction step S6, carrier gas extraction step S7, three-way valve second mode conduction step S8, and carrier gas injection into quantitative tube step S9.
[0078] The following describes the steps in the control method of the sample introduction device 100.
[0079] <Sample conduction step S1>
[0080] In this embodiment, the sample end valve port 22 is connected to the sample end 7, which stores the liquid sample to be analyzed, and the gas-liquid actuator 1 is connected to the actuator valve port 21. Referring to Figure 1, the gas-liquid actuator 1 is specifically a syringe, with one end of the conduit 14 connected to the syringe needle 13 and the other end connected to the actuator valve port 21. In the sample connection step S1, the actuator valve port 21 is connected to the sample end valve port 22 by adjusting the multi-port valve 2. At this time, the sample end 7 and the gas-liquid actuator 1 are in a connected state.
[0081] <Sample extraction step S2>
[0082] After the sample conduction step S1 is completed, the gas-liquid actuator 1 is controlled, that is, the syringe piston 12 is pulled, so that a negative pressure is formed in the syringe empty cylinder 11, so that the sample liquid stored at the sample end 7 passes through the sample end valve port 22 and the actuator valve port 21 in sequence until it is drawn into the syringe empty cylinder 11. When the stroke of the syringe piston 12 is completed, that is, when the sample liquid at the actuator valve port 21 stops flowing into the gas-liquid actuator 1, it means that the sample extraction step S2 is completed. At this time, the sample liquid drawn into the gas-liquid actuator 1 (i.e. the syringe empty cylinder 11) is the first predetermined amount of sample.
[0083] In this invention, the quantitative tube 3 has a fixed length, and the internal volume of the quantitative tube 3 is the sample injection volume. To ensure that the liquid in the quantitative tube 3 is full before the sample liquid enters the analysis tube 6, preferably, the volume of the first predetermined amount of sample is at least greater than the internal volume of the quantitative tube 3.
[0084] <Step S3 for opening the quantitative tube>
[0085] In this embodiment, after the sample extraction step S2 is completed, the valve port of the multi-way valve 2 is adjusted so that the quantitative tube valve port 25 is connected to the driver valve port 21. At this time, one end of the quantitative tube 3 is connected to the gas-liquid driver 1 through the quantitative tube valve port 25.
[0086] <Three-way valve first mode conduction step S4>
[0087] In the sample injection device 100 of this embodiment, the other end of the quantitative tube 3 is connected to the first port 41 of the three-way valve 4, and the third port 43 is connected to the waste gas recovery device 10 and the waste liquid recovery device 11 respectively. After the quantitative tube connection step S3 is completed or simultaneously with the quantitative tube connection step S3, the valve port of the three-way valve 4 is adjusted so that the first port 41 and the third port 43 of the three-way valve 4 are connected. At this time, the quantitative tube 3 is connected to the waste gas recovery device 10 and the waste liquid recovery device 11 through the multi-way valve 2.
[0088] <Sample injection step S5>
[0089] After the first mode of the three-way valve is turned on in step S4, the gas-liquid actuator 1, the metering tube 3, the waste gas recovery device 10, and the waste liquid recovery device 11 (external) are connected in sequence. Pushing the piston 12 of the syringe (gas-liquid actuator 1) compresses the volume of the syringe barrel 11, causing the sample liquid in the syringe barrel 11 to pass sequentially through the actuator valve port 21 and the metering tube valve port 25 until it flows into the metering tube 3. The piston 12 is continuously pushed to ensure that the sample liquid in the syringe barrel 11 fully enters the metering tube 3. When the sample liquid is detected flowing through the third port 43 to the waste liquid recovery device 11, it indicates that the metering tube 3 is full of sample liquid. At this point, step S5 of injecting the sample liquid into the metering tube is completed.
[0090] <Carrier Gas Activation Step S6>
[0091] After sample injection into the quantitative tube is completed in step S5, the volume of sample liquid in the quantitative tube 3 is the same as the internal volume of the quantitative tube 3. By controlling the fixed length of the quantitative tube 3, accurate quantification of the sample liquid can be achieved. In the carrier gas conduction step S6, the carrier gas end valve port 23 is connected to the carrier gas storage end 8. The valve port of the multi-way valve 2 is adjusted to make the actuator valve port 21 connected to the carrier gas end valve port 23. At this time, the carrier gas end 8 is connected to the gas-liquid actuator 1 through the multi-way valve 2.
[0092] <Carrier Gas Extraction Step S7>
[0093] After the carrier gas conduction step S6 is completed, the gas-liquid actuator 1 is controlled, i.e., the syringe piston 12 is pulled, creating a negative pressure inside the syringe barrel 11. This causes the carrier gas stored at the carrier gas end 8 to pass sequentially through the carrier gas end valve port 23 and the actuator valve port 21 until it is drawn into the syringe barrel 11. By observing the position of the end of the syringe piston 12 corresponding to the scale line on the wall of the syringe barrel 11 or by detecting the stroke of the syringe piston 12, the volume of carrier gas drawn into the syringe barrel 11 can be determined. At this point, the syringe barrel 11 contains a first predetermined amount of carrier gas, and the sample extraction step S2 is completed. The aforementioned carrier gas is used to push the sample liquid filled in the metering tube 3 out of the metering tube 3. To ensure that the sample liquid can be completely pushed out of the metering tube 3, preferably, the volume of the first predetermined amount of carrier gas is greater than the internal volume of the metering tube 3.
[0094] The volume of the first predetermined carrier gas is greater than the internal volume of the quantitative tube 3, which ensures that in the subsequent carrier gas injection step S9, the carrier gas can be used to fully and completely push the sample liquid accumulated in the quantitative tube 3 into the analysis tube 6, thereby ensuring the accuracy of the sample liquid injection volume.
[0095] <Three-way valve second mode activation step S8>
[0096] In this embodiment, the second port 42 of the three-way valve 4 is connected to the inlet of the sample injection block 5. After the carrier gas extraction step S7 is completed, the valve port of the three-way valve 4 is adjusted to make the first port 41 and the second port 42 of the three-way valve 4 open. At this time, the quantitative tube 3 is connected to the sample injection block 5 and the analysis tube 6 through the three-way valve 4.
[0097] <Carrier gas injection metering tube step S9>
[0098] After the second mode of the three-way valve is activated in step S8, the gas-liquid actuator 1, the quantitative tube 3, the sample injection block 5, and the analysis tube 6 are connected in sequence. Pushing the syringe piston 12 of the gas-liquid actuator 1 compresses the volume of the syringe empty cylinder 11, causing the first predetermined amount of carrier gas in the syringe empty cylinder 11 to pass sequentially through the actuator valve port 21 and the quantitative tube valve port 25 until it is pushed into the quantitative tube 3. The carrier gas then pushes out all the sample solution pre-accumulated in the quantitative tube 3, and the sample passes sequentially through the first port 41 and the second port 42, finally flowing into the sample injection block 5 and the analysis tube 6 for detection and analysis.
[0099] This embodiment, through the above steps, utilizes a fixed-length quantitative tube 3, using the internal volume of the quantitative tube 3 as the sample injection volume. This ensures that the sample injection volume of the injection device 100 is precise and controllable, and that the injection volume of the sample into the analytical device remains consistent across multiple injections. Therefore, the control method provided by this embodiment can guarantee the accuracy of the sample injection volume using a simple injection device 100 and through simple operation.
[0100] <Fourth Implementation Method>
[0101] In another control method for a sample introduction device 100 provided by the present invention, referring to FIG4, in addition to the steps of the third embodiment of the present invention, the execution steps of the control method further include: cleaning preparation step S10, quantitative tube connection step S3, and quantitative tube cleaning step S11.
[0102] The execution steps in this embodiment will be described below.
[0103] <Cleaning Preparation Step S10>
[0104] To avoid residual sample liquid in the pipeline of the injection device 100 after different batches of samples have passed through it for multiple analyses, which could interfere with the analysis results of the next batch of samples entering the injection device 100, this embodiment also includes a cleaning preparation step S10. Referring to Figures 2 and 4, the pure water end valve port 24 is connected to the pure water source 9 containing pure water. By adjusting the valve port of the multi-way valve 2, the driver valve port 21 is connected to the pure water end valve port 24. Controlling the gas-liquid actuator 1, i.e., pulling the syringe piston 12, creates a negative pressure inside the syringe barrel 11. This causes the pure water stored in the pure water source 9 to pass sequentially through the pure water end valve 24 and the actuator valve 21 until it is drawn into the syringe barrel 11. When the pure water stops flowing into the gas-liquid actuator 1 at the actuator valve 21, the volume of pure water drawn into the syringe barrel 11 can be determined by observing the position of the end of the syringe piston 12 corresponding to the scale line on the wall of the syringe barrel 11 or by detecting the stroke of the syringe piston 12. At this point, the syringe barrel 11 contains a first predetermined amount of pure water, and the cleaning step S10 is completed. To ensure that the pure water can fully clean the sample in the quantitative tube 3, preferably, the volume of the first predetermined amount of pure water in the gas-liquid actuator 1 is at least greater than the internal volume of the quantitative tube 3.
[0105] <Step S3 for opening the quantitative tube>
[0106] After the cleaning step S10 is completed, the metering tube connection step S3 is performed again. Specifically, the valve port of the multi-way valve 2 is adjusted so that the metering tube valve port 25 is connected to the actuator valve port 21. At this time, one end of the metering tube 3 is connected to the gas-liquid actuator 1. The valve port of the three-way valve 4 is then switched so that the first port 41 is connected to the third port 43.
[0107] <Quantitative tube cleaning step S11>
[0108] After completing step S3 of the quantitative tube connection, push the syringe piston 12 to allow the pre-accumulated pure water in the syringe to flow into the quantitative tube 3, cleaning the inside of the quantitative tube 3. The cleaned waste liquid flows sequentially through the first port 41 and the third port 43, and finally flows into the waste liquid recovery device 11. Alternatively, switch the three-way valve 4 to connect the first port 41 and the second port 42, push the syringe piston 12, and allow the pure water passing through the quantitative tube 3 to flow sequentially through the first port 41 and the second port 42 into the sample injection block 5 and the analysis tube 6, and finally flow out from the discharge port of the analysis tube 6 (not shown in the figure).
[0109] In other embodiments of the present invention, the sample liquid drawn in the gas-liquid actuator 1 can also be used to rinse the inside of the quantitative tube 3. Specifically, for the sample liquid to be analyzed, it is introduced into the sample injection device 100, and the sample conduction step S1, sample extraction step S2, quantitative tube conduction step S3, three-way valve first mode conduction step S4, and sample injection into the quantitative tube step S5 are executed in sequence, so that the sample liquid finally flows from the third port 43 into the waste liquid recovery device 11, thereby completing the rinsing of the inside of the quantitative tube 3 and reducing the dilution effect of the residual pure water on the sample solution after the pure water is used to clean the inside of the quantitative tube 3.
[0110] <Fifth Implementation Method>
[0111] This invention also provides a liquid monitoring and analysis instrument, including the aforementioned sample introduction device 100. By executing the above-described control method, when using this liquid monitoring and analysis instrument to detect and analyze liquid samples, the sample injection volume can be precisely quantitatively controlled, and the sample injection volume into the analysis device remains precisely consistent across multiple injections. Simultaneously, this liquid monitoring and analysis instrument can quickly switch between injection and cleaning modes to rapidly perform quantitative analysis and testing on multiple samples sequentially, avoiding interference between different samples during the injection and analysis process, thus ensuring the stability and accuracy of the analysis results.
[0112] The above are merely preferred embodiments of the present invention and are not intended to limit the present invention. Any modifications, equivalent substitutions, and improvements made within the spirit and principles of the present invention should be included within the protection scope of the present invention.
Claims
1. A sample introduction device, characterized by, include: Pneumatic-hydraulic actuators; The multi-port valve includes a driver valve port connected to the gas-liquid actuator, a sample end valve port connected to the sample end, a carrier gas end valve port connected to the carrier gas end, and a metering tube valve port. A metering tube, one end of which is connected to the valve port of the metering tube; The three-way valve includes a first port, a second port, and a third port. The first port is connected to the other end of the metering tube, and the third port is connected to the outside. The analysis tube is connected to the second port of the three-way valve.
2. The sample introduction device as described in claim 1, characterized in that, Also includes: The injection block is connected at one end to the second port of the three-way valve and at the other end to the analysis tube.
3. The sample introduction device as described in claim 1 or 2, characterized in that, The internal volume of the metering tube is the specified capacity.
4. The sample introduction device as described in claim 3, characterized in that, The gas-liquid actuator is either a syringe or a plunger pump.
5. The sample introduction device as described in claim 4, characterized in that, The volume of gas or liquid that the syringe or the plunger pump can extract is at least greater than the internal volume of the metering tube.
6. The sample introduction device as described in claim 1, characterized in that, The multi-way valve also includes a pure water end valve port, which is connected to an external pure water source.
7. A method for controlling a sample injection device, used in the sample injection device according to any one of claims 1-6, characterized in that, include, In the sample conduction step, the actuator valve port of the multi-way valve is controlled to connect with the sample end valve port. In the sample extraction step, the gas-liquid actuator is controlled to extract a first predetermined amount of sample into the gas-liquid actuator through the sample end valve port. The metering tube conduction step controls the connection between the metering tube valve port and the gas-liquid actuator; The first mode of the three-way valve is activated by controlling the activation of the first port and the third port of the three-way valve. In the sample injection metering tube step, the gas-liquid actuator is controlled to push the first predetermined amount of sample into the metering tube; The carrier gas conduction step involves controlling the connection between the driver valve port and the carrier gas end valve port of the multi-way valve. The carrier gas extraction step involves controlling the gas-liquid actuator to extract a first predetermined amount of carrier gas. The second mode of the three-way valve is activated by controlling the activation of the first port and the second port of the three-way valve. In the carrier gas injection metering tube step, the gas-liquid actuator is controlled to push the first predetermined amount of carrier gas to push the sample in the metering tube.
8. The control method for the sample introduction device according to claim 7, characterized in that, The volume of the first predetermined sample is greater than the internal volume of the quantitative tube.
9. The control method for the sample introduction device according to claim 8, characterized in that, The volume of the first predetermined amount of carrier gas is greater than the internal volume of the metering tube.
10. The control method for the sample introduction device according to claim 7, characterized in that, It also includes, Cleaning preparation step: Control the gas-liquid actuator to draw a first predetermined amount of pure water into the gas-liquid actuator through the pure water end valve port; The metering tube conduction step controls the connection between the metering tube valve port and the gas-liquid actuator; In the metering tube cleaning step, the gas-liquid actuator is controlled to push the first predetermined amount of pure water into the metering tube.
11. The control method for the sample introduction device according to claim 10, characterized in that, The volume of the first predetermined amount of pure water is greater than the internal volume of the metering tube.
12. A liquid monitoring and analysis instrument, characterized in that, Includes the sample introduction device as described in any one of claims 1-6.
13. The liquid monitoring and analysis instrument as described in claim 12, characterized in that, Perform the control method of the sample introduction device as described in any one of claims 7-11.