Continuous liquid sampling system and control method thereof
Technical Field
The invention belongs to the technical field of automatic detection, and particularly relates to a liquid sample injection system, in particular to a system which can realize continuous sample injection of a liquid sample, avoid damage of a suspended particle sample in liquid and has a complete matched cleaning and guaranteeing scheme.
Background
In many subjects such as life science, environmental science, marine science and medicine, it is important to detect and analyze soluble substances in liquid, such as chemical components of metal elements and inorganic salts, or suspended particles in liquid, such as biological particles of single cells, multicellular microorganisms, cell populations and non-biological particles of micro-plastic particles. Compared with the traditional detection and analysis mode, the detection flux and the processing speed of the flow-through liquid detection and analysis technology are obviously improved, and the improvement can reach the difference of orders of magnitude. Therefore, the flow-through liquid detection and analysis apparatus is widely used in research and production of various disciplines. In the flow-through liquid detection and analysis instrument, a liquid sample is analyzed and detected, the detected sample is pumped into the instrument and flows through a detection device, and a detection result is acquired. The transport and pressurization of the liquid sample is thus an important part thereof. The pump is a mechanical device commonly used in the current flow-through liquid detection and analysis instrument for realizing liquid sample conveying, and mainly uses a diaphragm pump, a peristaltic pump and a syringe pump in the prior art.
In particular, in indoor use scenarios such as laboratories, flow-through liquid detection analyzers are receiving attention because of their advantages such as high throughput and high detection speed. Through the flow-through liquid detection and analysis instrument, the samples cultured in a large scale in an indoor scene can be quickly, massively and efficiently detected and analyzed, and the state data of the cultured samples can be mastered. Meanwhile, when a large number of samples are collected in the outdoor environment, detection errors caused by changes due to overlong sample collection time can be avoided through rapid detection. Meanwhile, in order to improve the detection speed, the continuous sample introduction function is also an important requirement of the flow-through liquid analyzer.
Most of the existing flow-through liquid detection and analysis instruments with continuous sample introduction function are designed for detecting soluble (soluble) substances in liquid, such as phosphate, nitrate and other chemical components. The components exist in a form of being dissolved in liquid, and are not easily influenced by the structure and the working mode of the pump in the detection process, so that products capable of directly realizing the continuous sample feeding function, such as a peristaltic pump, are mainly selected for the instrument in the selection of the pump. However, for detecting insoluble suspended particles in a liquid, the influence on the suspended particles during the sample transportation process needs to be considered, so in an analysis instrument for detecting the suspended particle components in the liquid, certain requirements are imposed on the selection of a pump and the structure of a liquid path. At present, peristaltic pumps and diaphragm pumps are mostly adopted as water pumping units in detection and analysis instruments for realizing continuous sample injection in the market. However, in the actual product, the two pumps are not suitable for use directly in front of (upstream) the detection area due to their own structure and operation principle limitations. In the diaphragm pump, it is necessary to control the suction and discharge of the liquid by a check ball valve. Because of the existence of the ball valve, in the case that a fragile sample, such as plankton, microorganism and other tiny suspended particulate matter insoluble in liquid, exists in the liquid sample, when such liquid sample is conveyed, the ball valve may cause damage to the fragile sample in the liquid, resulting in fragmentation and other consequences of the observation object. In addition, a certain shearing force is generated in the conveying process of the diaphragm pump, and the fragile sample can be damaged. Similarly, during the liquid sample transportation process using the peristaltic pump, due to the roller compaction of the peristaltic pump on the flexible tube, if the liquid contains a fragile sample that is insoluble in the liquid, the liquid may be damaged by the extrusion during the operation of the peristaltic pump, which also results in inaccurate observation. Taking the detection and analysis of phytoplankton as an example, phytoplankton belongs to suspended particulate matters in liquid in a detection sample, and various phytoplankton exist in various existing forms such as single cells, chain-like multicellular cells, cell populations and the like. If the diaphragm pump or the peristaltic pump is used as a water pumping unit, the structures and the existing forms of chain-shaped and group cells are easily damaged in the liquid conveying process, single cells with larger particle sizes are broken due to extrusion and cannot keep the original forms, and therefore the accuracy of detection results is affected.
According to the above description, in the detection and analysis of the suspended particles in the liquid, in order to avoid inaccurate detection results caused by damage to the suspended particles during detection, the selection of the pump and the position of the pump in the liquid path are very important. Some products currently in the market have a post pump as a solution to protect the suspended particles during design. For example, in the FlowCAM series flow cytometry system manufactured by Fluid Imaging, a peristaltic pump is used in the apparatus for analyzing aquatic microorganisms to control the flow rate and flow velocity and to realize continuous sample injection, and the apparatus is installed behind the detection area. The sample passes through the detection area and then passes through the peristaltic pump body, and the sample after detection is damaged. However, the use mode of the pump with damage to suspended particles at the downstream of the detection area only solves the problem of no damage during detection, and does not consider the damage after sample detection. In the practical application of the flow-through detection and analysis instrument, the detection is often recycled after detection, and other subsequent detection works are performed, such as High Performance Liquid Chromatography (HPLC), sequencing, manual microscopic examination and the like. Therefore, recovery of the sample is essential. In addition, when the sample to be detected is precious or difficult to obtain repeatedly and needs to be recycled for multiple times, the existing peristaltic pump rear-mounted mode can not meet the requirement of nondestructive detection.
Besides the influence of the structure of the pump body, the conveying modes realized by the pumps of different types can also influence the detection to a certain extent. Due to the working principle of the peristaltic pump and the diaphragm pump, the stable conveying of the sample can be influenced by the fluid pulsation generated when the peristaltic pump and the diaphragm pump work at low flow. The conveying mode with the pulse can influence the accurate quantification of the conveyed samples, and the liquid conveying sample introduction with stable flow velocity can not be realized. The non-stationary sample introduction can seriously affect some detections requiring precise measurement, such as the accuracy of light intensity and frequency detection signals and the image quality of imaging detection. This deterioration in the detection information can in turn severely degrade the accuracy of the flow-through liquid detection and analysis instrument. Therefore, pulsed pumps such as diaphragm pumps and peristaltic pumps do not meet the requirements of flow-through liquid detection and analysis instruments for smooth sample transport.
In order to realize smooth and nondestructive sample feeding work, a syringe pump is generally adopted as a water pumping device. Referring to the description and the attached drawing fig. 1, the injection pump mainly comprises a stepping motor 101, a driver, a screw rod 102 and an injector 105. When the injection pump works, the driver sends out a control command to enable the stepping motor 101 to rotate, the rotating motion of the stepping motor 101 can be converted into the linear motion of the nut 103 through the screw rod 102, and then the piston 104 of the injector 105 is pushed to perform injection and extraction work. The injection pump driver can drive the screw rod 102 through the accurate control of the stepping motor 101, and push the injector piston 104 to stably work at a constant speed, so that the high-precision stable conveying of the liquid sample is realized. Meanwhile, the pump body of the injection pump is simple in structure, has no structure for damaging the sample, does not generate shearing force in the conveying process, has no damage to the conveyed liquid sample, and is an ideal conveying mode for the fragile sample. Compared with the problems of the diaphragm pump and the peristaltic pump, the injection pump has the characteristics of high precision, stable and lossless fluid transmission and the like, so that the injection pump becomes an ideal mode for conveying suspended particle samples in liquid samples.
However, due to the limitation of the working principle of the syringe pump, the injection process and the extraction process need to be completed intermittently, and the single syringe pump used in the current flow-through liquid detection and analysis instrument cannot realize continuous liquid delivery. Thus, the use of a single syringe pump limits its application when continuous feeding is required. When the flow-through liquid detection and analysis instrument for suspended particles in liquid is applied to a continuous sampling scene, continuous sampling can be realized by ensuring, and protection of the suspended particles in the liquid and stable conveying of samples need to be considered. Therefore, the requirement on a sample feeding system is more severe, and the stability, continuity and flux of sample conveying need to be coordinated by various devices such as light, machinery, electricity and the like.
In addition, it is worth noting that in the sample injection system, besides the water pumping system, the design of the liquid path structure and the cleaning guarantee mechanism is also very important. First, with regard to the design of the pipeline, when the flow-through liquid detection and analysis instrument is used to perform detection and analysis on soluble substances in a liquid sample, because the detection object exists in a form of being dissolved in water, the detection process is not affected by the structure of the sample injection device. Therefore, in such an apparatus for detecting a soluble substance, a small-diameter or diameter-reduced pipe is generally used in selection and design of a pump valve and a liquid path in order to reduce the load on the liquid path in the apparatus and to reduce the cost of the apparatus, and the influence of the apparatus structure and the liquid path design on the detection of suspended particles in a liquid is not considered. However, when detection analysis of suspended particulate matter such as phytoplankton and the like in a liquid sample is required, these particulate matter are suspended in the liquid sample, and there are large-particle-size individuals or large-particle-size populations such as chain-like or cluster-like cell populations. To maximize sample integrity and authenticity, large bore pump valves and piping are often required to ensure proper passage of the suspended particulate matter.
Besides the structural design of the liquid path, a cleaning guarantee mechanism is also an important link for ensuring the normal work of the instrument. In the indoor environment, often need detect to different samples, there is the switching problem of sample. In the switching process of different samples, after the last sample detection is completed, the instrument needs to be cleaned comprehensively, and the detection error caused by the mixing of the previous sample and the next sample caused by the residue of the previous sample is avoided. During the sample transportation process of the instrument, air bubbles in the sample often adhere to the detection area of the instrument, which can seriously affect the detection result based on the optical principle. Therefore, for bubbles attached to the detection area during sample injection, a removal mechanism and design are required to ensure the accuracy of the detection result.
To sum up, the flow-through liquid detection and analysis instrument for continuous sampling of suspended particles in liquid needs to meet multiple technical requirements of continuous sampling, nondestructive protection of tiny particles, stable sampling, cleaning guarantee and the like. The injection pump is an ideal water pumping system of the flow-through liquid detection and analysis instrument due to the characteristics of high precision, stability and lossless delivery. However, due to the limitation of the working principle of the syringe pump, no continuous-working flow-through detection instrument based on the syringe pump is applied to the imaging detection of the biological particles at present. Meanwhile, the existing flow-through detection instrument usually lacks a liquid path and a control design thereof under the condition of suspended particulate matters in a liquid sample, for example, the absence of pipeline design and cleaning guarantee measures can cause that the instrument cannot be normally applied to a specific monitoring scene. Therefore, the realization of a continuous sampling system based on a syringe pump and suitable for suspended particle monitoring is of great significance for flow-through liquid detection and analysis instruments using optical principles as detection means.
Disclosure of Invention
In order to meet the requirements of indoor working environment of instruments and solve the problems of the existing flow-through liquid detection and analysis instrument, the invention designs a system for protecting continuous sample introduction of samples in a mode of alternatively working by a plurality of injection pumps, which is suitable for detection and analysis of micro particles. When one injection pump is in an injection sample feeding state, the other injection pump can wait for taking over the sample feeding work after extracting the sample; when the prior injection pump finishes sample injection through injection action, the design of the corresponding valve unit is utilized, the sample injection pipeline can be switched to the injection pump which finishes sample injection in addition in a very short time, and the sample injection is continued; at this point, the pump that completed the injection can then draw the next tube of sample to wait. Therefore, the injection pumps can complete stable, continuous and lossless sample feeding operation by alternately working. In addition, the invention also combines the structure of a plurality of injection pumps to design a perfect liquid path cleaning and bubble removing guarantee scheme, thereby ensuring the completeness of instrument cleaning. And through using the liquid storage ring, the phenomenon that the sample is remained and precipitated in the injection pump due to the contact of the injection pump and the tested sample is avoided, and the easy cleaning performance and the durability of the sample feeding system are enhanced. Meanwhile, the perfect cleaning function can prevent the sample with recovery requirement used in the experiment from being polluted in the detection process.
The continuous liquid sampling system comprises two or more injection pumps, a control unit, a valve unit and a detection chamber; the liquid outlet of each injection pump can be communicated with the corresponding interface of the valve unit, and the device is characterized in that the control unit is electrically connected with each injection pump and the valve unit, and the valve unit can communicate different injection pumps with the detection chamber or the sample source in a time-sharing manner under the control of the control unit; for each syringe pump, the control unit controls the syringe pump to draw a sample from the sample source when the syringe pump is in communication with the sample source, and controls the syringe pump to push the sample to the detection chamber when the syringe pump is in communication with the detection chamber. Wherein the valve unit comprises an N-channel rotary valve and a multi-channel rotary valve; the N-channel rotary valve has a plurality of ports as follows: a C interface corresponding to and communicated with the multi-channel rotary valve, a detection chamber interface corresponding to and communicated with the detection chamber, and two or more injection pump interfaces corresponding to each injection pump; the multi-channel rotary valve comprises a liquid path inlet communicated with the C interface in the N-channel rotary valve and a liquid path outlet corresponding to and communicated with a sample source; the control unit can switch the different injection pump interfaces to be communicated with the C interface of the N-channel rotary valve, so that different injection pumps are controlled to be communicated with the liquid path inlet of the multi-channel rotary valve at different time periods; the control unit can switch the different syringe pump interfaces to be communicated with the detection chamber interface of the N-channel rotary valve, so that different syringe pumps are controlled to be communicated with the detection chamber at different time intervals.
Further, the system also includes a cleaning unit comprising a plurality of cleaning interfaces; each cleaning interface is provided with a corresponding liquid path outlet which is communicated with the multi-channel rotary valve. With an N-channel rotary valve, all external ports and any one pump can be considered to be connected through the same port. Each pump can be communicated with the multi-channel rotary valve only by being connected with the N-channel rotary valve, and further communicated with all the interfaces on the multi-channel rotary valve. Thus greatly simplifying the complexity of the fluid path in the system.
The system further comprises a bubble removing unit, wherein the bubble removing unit comprises a monitoring unit, and the monitoring unit is used for monitoring whether the detection chamber has bubbles with influence on the detection effect; one end of the detection chamber is also provided with an opening to enable liquid to be pumped from one end of the detection chamber to push the bubbles away.
The bubble removing unit also comprises a bubble removing interface, and the bubble removing interface is provided with a corresponding and communicated liquid path outlet in the multi-channel rotary valve; the opening can be communicated with the bubble removal interface under the control of the control unit. Alternatively, the bubble removal unit further comprises a Y-shaped flow path valve; a liquid path outlet of the multi-channel rotary valve, which corresponds to the detection chamber, is communicated with a first interface of the Y-shaped flow path valve, a second interface of the Y-shaped flow path valve is connected with a normal sample inlet of the detection chamber, and a third interface of the Y-shaped flow path valve is connected with the opening at the bottom of the detection chamber; the control unit can control whether the liquid path of the Y-shaped flow path valve is communicated with the first interface and the second interface or the first interface and the third interface.
Regarding the cleaning unit, further the cleaning interface comprises a purified water interface communicated with the purified water container, a cleaning agent interface communicated with the cleaning agent container, a disinfectant interface communicated with the disinfectant container and an air interface communicated with the outside air. Alternatively, the cleaning interface may be in communication with two or more sub-cleaning interfaces, and the sub-cleaning interfaces may further include a purified water interface for communicating with a purified water container and an air interface for communicating with outside air.
In order to avoid sample residue, precipitation and prolong the service life of the system, the injection pumps caused by inaccurate detection caused by sample mixing and long-time sample contact are prevented from being corroded, the liquid outlets of the two or more injection pumps are also provided with a liquid storage ring, one end of the liquid storage ring is connected with the liquid outlet of the injection pump, and the other end of the liquid storage ring is connected to the inlet of a multi-channel rotary valve liquid path of the corresponding injection pump in the valve unit or the injection pump interface of the N-channel rotary valve. The liquid storage ring is formed by spirally winding a hard tube. Preferably, the volume of the reservoir ring is slightly greater than the volume of the pump chamber of the attached syringe pump plus a small amount of air in the space.
Corresponding to the above-described system, a related control method of the system is explained as follows. The control method for continuous sample injection comprises the following steps:
s1, initializing the system;
s2, switching a liquid path inlet of the multi-channel rotary valve to be connected with a liquid path outlet corresponding to a sample source; the N-channel rotary valve is switched to communicate the C interface with a syringe pump interface, so that a syringe pump is communicated with the sample source;
s3, controlling the injection pump in the step S2 to pump the sample;
s4, judging whether the sample extraction of the syringe pump for extracting the sample in the step S3 is finished;
s5, keeping the liquid path of the multi-channel rotary valve unchanged; controlling the N-channel rotary valve to communicate the injection pump interface corresponding to the injection pump which finishes the sample extraction with the detection chamber interface so as to communicate the injection pump with the detection chamber, and to communicate the injection pump interface corresponding to the other injection pump except the injection pump which finishes the sample extraction with the C interface so as to communicate the injection pump with the sample source;
s6, controlling a syringe pump communicated with the detection chamber to inject a sample into the detection chamber, and controlling the syringe pump communicated with a sample source to extract the sample from the sample chamber;
s7, judging whether the injection pump for injecting the sample finishes sample injection and judging whether the injection pump for extracting the sample finishes sample extraction;
and S8, judging whether sample introduction is needed, if so, returning to the step S5, and if not, ending the sample introduction process.
Preferably, the control method further comprises a bubble monitoring and removal process performed according to the following steps:
BS1, judging whether bubbles influence the detection accuracy;
BS2, when air bubbles exist, the currently working injection pump stops working, and the Y-shaped flow path valve is switched to an air bubble removal liquid path;
BS3 and the injection pump continue to carry out sample injection, and bubbles influencing the detection accuracy in the detection area are removed through a bubble removal liquid path;
BS4, the injection pump stops working, the Y-shaped flow path valve is switched to the detection liquid path,
and the BS5 and the injection pump continue to perform sample injection work.
In addition, the bubble removal can be realized by the following process:
CS1, judging whether bubbles influence the detection accuracy;
CS2, when bubbles exist, the current working injection pump stops working and executes one or more times of back pumping operation;
CS3, judging whether the bubbles affect the detection accuracy, if not, recovering the normal sample introduction.
Further, the control scheme is also applicable to the following cleaning control steps:
s50, judging whether the sample injection process is finished or not, and executing a cleaning process;
s51, controlling the multi-channel rotary valve to switch channels, and enabling a liquid path inlet of the multi-channel rotary valve to be communicated with a liquid path outlet corresponding to the Mth cleaning interface; controlling the C interface of the N-channel rotary valve to be communicated with an injection pump interface so as to communicate the injection pump with the Mth cleaning interfaces;
s52, controlling a syringe pump communicated with the Mth cleaning interface to pump the cleaning reagent from the Mth cleaning interface;
s53, judging whether the injection pump which extracts the cleaning reagent from the Mth cleaning interface finishes extracting the cleaning reagent;
s54, controlling the N-channel rotary valve to communicate the injection pump interface corresponding to the injection pump which just extracts the cleaning reagent with the detection chamber interface so as to communicate the injection pump with the detection chamber; controlling the syringe pump interface corresponding to another syringe pump except the syringe pump which just pumps the cleaning reagent to be communicated with the interface C so as to communicate the other syringe pump with the Mth cleaning interface;
s55, controlling a syringe pump communicated with the detection chamber to push the cleaning reagent into the detection chamber; controlling a syringe pump communicated with the Mth cleaning interface to start to pump cleaning reagent;
s56, judging whether the injection pump for pushing the cleaning reagent finishes pushing or not and whether the injection pump for extracting the cleaning reagent finishes extracting the cleaning reagent or not;
and S57, judging whether all the required cleaning reagents are pushed completely, if so, ending the cleaning process, otherwise, turning to the step S54 when M is equal to M + 1.
In the control method, it is preferable that the injection pump injects the sample or the cleaning agent into the detection chamber at a rate lower than a rate at which the sample or the cleaning agent is withdrawn from the sample chamber.
Alternatively, the operation of determining whether the syringe pump for injecting the sample or the washing reagent has completed injecting the sample, and the operation of determining whether the syringe pump for extracting the sample or the washing reagent has completed extracting the sample are replaced by the operation of passing a fixed time interval.
The invention also provides a flow-through liquid detection and analysis instrument which uses the continuous liquid sampling system and the continuous sampling system can use the control method.
Compared with the prior art, the continuous sample introduction system and the flow-through liquid detection instrument using the same designed by the invention can overcome the problem that continuous sample introduction cannot be realized by a single injection pump, and realize continuous, accurate and stable sample introduction on the premise of protecting vulnerable samples. Because a plurality of injection pumps are used, the adaptability of system failure is improved, and in the case of injection pump failure, other injection pumps can be used as backup pumps to continue working. Meanwhile, the whole sample feeding system is more compact in structure and smaller in volume based on the selection and design of the pump valve, so that the system can be suitable for more scenes with requirements on the volume. Most importantly, the invention designs the cleaning scheme and the bubble removing scheme, and the bubble removing function ensures that the system can timely process bubbles influencing detection, thereby avoiding the influence on the detection result and greatly improving the detection precision of the instrument. The liquid storage ring also has the advantages of simple structure, easy cleaning and convenient replacement, and the injection pump can realize non-contact pumping of samples by using the liquid storage ring, thereby avoiding the influence on the instrument detection result and the loss of system equipment caused by the reasons of sample residue and the like due to the precipitation in the pump possibly appearing because of the long-term contact between the samples and the injection pump. Therefore, compared with the prior art, the continuous sampling system and the flow-through liquid detection instrument using the same have a better sample application range, are beneficial to obtaining better detection precision, have longer service life and have better user experience on the whole.
Drawings
FIG. 1: the structure of the injection pump in the prior art is schematic;
FIG. 2: a schematic structural diagram of a continuous sample introduction system;
FIG. 3: a continuous sample introduction control flow chart;
FIG. 4: a cleaning control flow chart;
FIG. 5: and (5) an integrated interface structure schematic diagram.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the technical solutions of the present invention will be clearly and completely described below with reference to the specific embodiments of the present invention and the accompanying drawings. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The invention designs a continuous sample introduction system which can be suitable for a flow-through liquid detection instrument. To avoid damage to the tiny particles or tiny aquatic organisms in the liquid sample, a syringe pump is used to accomplish the delivery of the liquid sample. In particular, two or more syringe pumps are used, and a valve unit is combined to alternately communicate one of the syringe pumps with the detection chamber. The liquid outlet of each injection pump can be communicated with the corresponding interface of the valve unit, the injection pumps can be communicated with the detection chamber or the sample source in a time-sharing mode through switching of the valve units, the system control unit is electrically connected with the injection pumps and the valve units respectively, so that regulation and control of the injection pumps and the valve units are achieved, conveying and extraction of liquid samples are completed, two or more injection pumps push the liquid samples when matched with each other, and continuous conveying of the liquid samples to the detection chamber is achieved.
Meanwhile, the continuous sampling system is also provided with a cleaning unit and a bubble removing unit. The cleaning unit comprises a plurality of cleaning interfaces and cleaning liquid paths corresponding to the cleaning interfaces. The cleaning interfaces realize the respective communication of the cleaning liquid paths corresponding to the cleaning interfaces with the pure water bottle, the cleaning bottle, the disinfection bottle and the external air. A plurality of cleaning solution way can communicate with the corresponding export of valve unit respectively to the realization is respectively with pure water in the pure water bottle, the cleaner in the cleaning bottle, disinfectant and the outside air in the disinfection bottle extract the syringe pump and then the propelling movement to the detection room in, so realize the washing of the whole liquid way of sampling system in succession. The bubble removing unit is used for monitoring and removing bubbles influencing the detection accuracy in real time. The bubble removing unit comprises an opening at one end of the detection chamber and a bubble removing interface, wherein a pipeline is communicated between the opening and the bubble removing interface, and the bubble removing interface can be communicated with a corresponding outlet of the valve unit or other pumping units, so that a sample or water is pushed from one end of the detection chamber to the inside of the detection chamber to push away bubbles staying in the inside of the detection chamber.
Therefore, the continuous sample introduction system not only can continuously convey liquid samples to the detection chamber and avoid fragile samples in the liquid samples from being damaged, but also has the functions of efficient and complete automatic cleaning of a liquid path and removal of bubbles in the detection chamber, and is particularly suitable for analysis instruments such as a flow-through liquid detector in an indoor environment or liquid conveying equipment with high requirements on liquid state maintenance.
Specifically, refer to fig. 2 of the specification, which is a schematic structural diagram of the continuous sampling system of the present invention. In the present embodiment, the system is composed of a control unit 1, two syringe pumps a and B, a valve unit 2, a detection chamber 4, a cleaning unit 5, and a bubble removing unit 6. In this embodiment the system further comprises a sample chamber 3 as a sample source, especially in a laboratory environment, the sample chamber 3 being common and versatile. However, it will be readily understood by those skilled in the art that the sample chamber 3 merely represents a source of the sample and that the sample chamber 3 may be replaced by other sources of the sample. Further, the valve unit 2 specifically includes a two-way type flow-path valve 9 corresponding to both the syringe pumps a and B and a multi-path rotary valve 10 corresponding to the two-way type flow-path valve 9. In order to prevent the syringe pump from being corroded, it is preferable to further use a liquid reservoir ring, i.e., the liquid outlets of the syringe pumps a and B are connected to one end of the liquid reservoir rings 8A and 8B, respectively. And the other ends of the liquid storage rings 8A and 8B are connected to a two-way type flow path valve 9. The above-mentioned liquid reservoir rings 8A and 8B are used in particular by a hard tube helically coiled, preferably with an outer diameter not greater than the outer diameter of the pump chamber of the syringe pump. The volume of the liquid storage ring is preferably slightly greater than the volume of the syringe pump chamber and the total volume of a small volume of air, and is particularly selected from a corrosion-resistant and non-deformable material, such as a metal material or PTFE. Before the sample injection system works, pure water with the same volume as the pump cavities of the injection pumps A and B is stored in the liquid storage rings 8A and 8B respectively, one end of the pure water is in contact with the liquid outlet of the injection pump, and a small section of air is reserved at the other end of the pure water. Thus, when the injection pumps A and B draw samples, the pump cavities of the injection pumps A and B are filled with the section of pure water, and the liquid sample can be separated from the pure water in the injection pumps by the small section of air. Thus, when the syringe pump is operated, the withdrawn liquid sample or other cleaning liquid will be stored in the reservoir rings 8A and 8B without entering the pump chambers of the syringe pumps a and B. Alternatively, depending on the type of liquid sample to be injected, inert gas or other fluid immiscible with the liquid sample, such as oil, may be used in the liquid storage ring instead of pure water or air. Due to the use of the liquid storage ring, the possibility of corrosion of the pump cavity of the injection pump is reduced, and the liquid storage ring is low in cost and convenient to replace, so that the service life and the application range of the sample injection system are prolonged.
Further, the structure of the two-way flow-path valve 9 refers to the corresponding part in the attached figure 2 of the specification, and the two-way flow-path valve has four interfaces of (i), (ii) and (C). The two-way flow valve 9 has two connection states, and the interface C can be respectively communicated with the interfaces firstly and thirdly. In the two states, the paths (solid line state in the two-way type flow path valve 9 shown in the figure) and the paths (not shown) are formed (r-C and C-C), respectively. The first, the third and the fourth cannot be communicated with each other.
One end of two liquid storage rings 8A and 8B respectively corresponding to the injection pumps A and B is connected with the corresponding injection pump, and the other end is respectively communicated with two ends of the first and third two-way flow path valves. A liquid channel inlet of the multi-channel rotary valve 10 is connected with a connector C of a two-way type flow channel valve 9, a connector of the detection chamber 4 is connected with a connector II of the two-way type flow channel valve 9, and a Y-type flow channel valve 611 is further arranged between the connector of the detection chamber 4 and the connector II of the two-way type flow channel valve 9 in the figure in order to achieve the bubble removing function. The interface of the sample chamber 3 is connected with a corresponding liquid path outlet in the multi-channel rotary valve 10. Therefore, the control unit 1 controls whether the injection pumps A and B are communicated with the detection chamber 4 or the sample chamber 3 or other interfaces by controlling the two-way flow-path valve 9 and the multi-channel rotary valve 10, and realizes the continuous sample introduction of the liquid sample to the detection chamber 4 by matching with the control of the control unit 1 on the injection pumps A and B. The control unit 1 can adopt the existing control method for controlling the injection pumps A and B, namely controlling the injection and the extraction of the injection pumps by a stepping motor; the control unit 1 controls the two-way type flow-path valve 9 and the multi-path rotary valve 10 by controlling the rotors of the respective valves to change the communication of the fluid paths thereof.
In this embodiment, the control flow performed by the control unit 1 to realize continuous sample injection is shown in fig. 3 in the specification. When the continuous sampling system of this embodiment starts to operate, step S1 initializes the pumps and valves in the system. Then the control unit 1 executes step S2, the multi-channel rotary valve 10 rapidly switches the fluid path to connect the fluid path inlet with the fluid path outlet of the corresponding sample chamber 3, and the two-way flow valve 9 switches to the communication state of C-first and C-third. Subsequently, in step S3, the syringe pump a pumps the liquid sample into the liquid storage ring 8A for temporary storage through the sample chamber 3 interface, the multi-channel rotary valve 10, and the C-r flow path of the two-way flow path valve 9. The control unit 1 determines in step S4 whether the sampling operation of the syringe pump a is completed. When the sampling operation is judged to be completed, step S5 is executed to switch the two-way flow valve 9 to the communication state of (r) -C and (C) -and the fluid path of the multi-path rotary valve 10 remains unchanged. In this manner, in step S6, the control unit 1 controls the syringe pump a to start pushing the piston, and sends the liquid sample in the liquid storage ring 8A to the detection chamber 4 through the (r) -c flow path of the two-way flow path valve 9. Meanwhile, the control unit 1 also controls the injection pump B to start sampling, and a liquid sample enters the liquid storage ring 8B for temporary storage through the sample chamber 3 interface, the multi-channel rotary valve 10 and the C-third flow path of the two-way flow path valve 9. In step S7, the control unit 1 performs a determination operation to determine whether the sampling by the syringe pump a is completed and to determine whether the sampling by the syringe pump B is completed. When both of the above-described judged operations are completed, the control unit 1 switches the two-way flow valve 9 to the communication of (C) and (C) in step S8. After the above switching is completed, in step S9, the control unit 1 controls the syringe pump B to start pushing the liquid sample in the liquid storage ring 8B to enter the detection chamber 4 through the two-way flow valve 9, and the syringe pump a starts to extract the sample again through the sample chamber 3 interface, the multi-channel rotary valve 10, and the C-one flow path of the two-way flow valve 9 to enter the liquid storage ring 8A for temporary storage. In step S10, the control unit 1 determines again whether the sampling operation of the syringe pump a is completed and the sampling operation of the syringe pump B is completed. Then, in step S11, it is determined whether sample injection is needed, and when continuous sample injection is needed, the control flow of the control unit 1 returns to step S5 to repeat the above operations to continue sample injection until the needed sample injection is completed. Thus, the injection pump A and the injection pump B work alternately, and continuous sample introduction of the detection chamber 4 is realized. After the sample introduction is finished, the subsequent cleaning operation can be executed.
Although separate judgments are made as to whether the sample introduction is completed and the sample extraction is completed in steps S4, S7, and S10, the control unit 1 may alternatively not make the judgments, but perform steps S5, S8, and S11 after a set fixed time interval has elapsed. The fixed time interval is more than or equal to the time required by the injection pump to finish one-time sample injection.
Further, optionally, a judgment on whether the required sample injection is completed may also be added after the step S7. Therefore, after each injection pump finishes one-time sample injection, the determination of whether all sample injections are finished is made, and the judgment is made after all injection pumps finish one-time sample injection, so that excessive sample injection to the detection chamber 4 can be avoided.
It should be emphasized that the switching time between the liquid paths in the two-way flow path valve 9 is also very short, and the switching speed can reach hundreds of milliseconds, so that the whole set of sample injection system can realize the approximate continuous sample injection only by completing the simple liquid path switching, and the design in the valve unit 2 can also simplify the design and control flow of the sample injection system. After the liquid sample is transferred to the detection chamber 4 for detection, it may be transferred to a waste chamber 7 connected to the detection chamber 4 for subsequent processing. When the sample is more valuable or the liquid sample needs to be used repeatedly according to the requirement of detection, the detection chamber 4 can also be connected with the sample chamber 3 through a corresponding pipeline, and the detected liquid sample is conveyed back to the sample chamber 3.
When the required sample injection is completed, the sample injection system of the embodiment can also complete the automatic cleaning function. Referring to fig. 2 of the specification, the cleaning unit 5 specifically includes a purified water interface 51, a cleaning agent interface 52, a disinfectant interface 53, and an air interface 54. Each of the above-mentioned ports corresponds to one of the fluid outlets of the multi-channel rotary valve 10, and each of the ports is connected to the corresponding fluid outlet of the multi-channel rotary valve 10 by a pipeline, so that what reagents are used for washing are controlled by the multi-channel rotary valve 10. In this embodiment, the above-mentioned interface and the pipeline of the liquid outlet can be very short, and the two-way flow valve 9 is selected to communicate with different injection pumps, so the whole set of sample introduction system can have a smaller volume.
When the sample feeding system executes cleaning operation, one pump can be used for cleaning through switching of the multi-channel rotary valve, and a plurality of pumps can be used for cleaning by combining control of the multi-channel rotary valve and control of the two-way flow path valve. Referring to fig. 4 in the specification, a main cleaning control flow chart in the present embodiment is shown, and the cleaning flow mainly includes:
s50, judging whether the sample injection process is finished or not, and executing a cleaning process;
s51, controlling the multi-channel rotary valve to switch channels, and enabling a liquid path inlet of the multi-channel rotary valve to be communicated with a liquid path outlet corresponding to the Mth cleaning interface; controlling the C port of the N-channel rotary valve (e.g., the two-channel rotary valve in this embodiment) to communicate with a syringe pump port, thereby communicating the syringe pump with the mth purge ports;
s52, controlling a syringe pump communicated with the Mth cleaning interface to pump the cleaning reagent from the Mth cleaning interface;
s53, judging whether the injection pump which extracts the cleaning reagent from the Mth cleaning interface finishes extracting the cleaning reagent;
s54, controlling the N-channel rotary valve to communicate the injection pump interface corresponding to the injection pump which just extracts the cleaning reagent with the detection chamber interface so as to communicate the injection pump with the detection chamber; controlling the syringe pump interface corresponding to another syringe pump except the syringe pump which just pumps the cleaning reagent to be communicated with the interface C so as to communicate the other syringe pump with the Mth cleaning interface;
s55, controlling a syringe pump communicated with the detection chamber to push the cleaning reagent into the detection chamber; controlling a syringe pump communicated with the Mth cleaning interface to start to pump cleaning reagent;
s56, judging whether the injection pump for pushing the cleaning reagent finishes pushing or not and whether the injection pump for extracting the cleaning reagent finishes extracting the cleaning reagent or not;
and S57, judging whether all the required cleaning reagents are pushed completely, if so, ending the cleaning process, otherwise, turning to the step S51 when M is equal to M + 1.
Specifically, M is, for example, an integer from 1 to 4, the 1 st cleaning interface is a purified water interface 51, the 2 nd cleaning interface is a cleaning agent interface 52, the 3 rd cleaning interface is a disinfectant interface 53, and the 4 th cleaning interface is an air interface 54.
The control flow of the cleaning is described in further detail below. If the control unit 1 determines that the injection pump B does not need to continue to perform the sample injection after the injection pump a completes the current sample injection, the cleaning operation is performed. In step S51, the two-way flow valve 9 is switched to communicate with the first and second valves to prepare the syringe pump B to take over the syringe pump a for sample injection, and the multi-way rotary valve 10 is switched to communicate with the inlet of the fluid path corresponding to the cleaning agent port 52. Subsequently, in step S52, the syringe pump a starts to pump the cleaning agent into the reservoir ring 8A, while the syringe pump B continues to feed the sample into the detection chamber 4. The control unit 1 determines in step S53 whether the cleaning agent pumping by the syringe pump a is completed and simultaneously determines whether the sample injection by the syringe pump B is completed. When both of the above-described judged works are completed, step S54 is executed, and the control unit 1 switches the two-way type flow valve 9 to the communication of C-C and (r) -C without the change of the multi-way rotary valve 10. In this manner, in step S55, the control unit 1 may control the syringe pump B to start pumping the cleaning agent into the liquid reservoir ring 8B, and may control the syringe pump a to push the cleaning agent into the detection chamber 4 to start the cleaning operation of the detection chamber 4 and the liquid path. In step S56, the control unit 1 determines whether the injection of the cleaning agent by the syringe pump a is completed and whether the extraction of the cleaning agent by the syringe pump B is completed. When the above two operations are completed, in step S57, the two-way flow-path valve 9 is switched to the communication between (C) - (r) - (g), and the multi-path rotary valve 10 is switched to the communication between the inlet of the liquid path and the outlet of the liquid path corresponding to the disinfectant port 53. Thus, in step S58, the syringe pump a starts to pump the disinfectant into the liquid storage ring 8A, and the syringe pump B pushes the cleaning agent in the liquid storage ring 8B into the detection chamber 4 to continue the cleaning operation. Step S59 judges that the syringe pump a finishes extracting the disinfectant, and after judging that the syringe pump B finishes pushing the cleaning agent, in step S510, the two-way flow valve 9 is switched to be communicated with C-C and (r) -C, while the liquid path of the multi-path rotary valve 10 remains stationary. Thus, in step S511, the injection pump a starts to push the disinfectant to the detection chamber 4, so as to sterilize the detection chamber 4 and the liquid path, and meanwhile, the injection pump B may start to pump the disinfectant into the liquid storage ring 8B. Similarly, after the injection pump a finishes the injection of the disinfectant and the injection pump B finishes the extraction of the disinfectant in step S512, step S513 is executed to switch the multi-channel rotary valve 10 to have its fluid channel inlet communicated with the fluid channel outlet corresponding to the purified water interface 51, and to switch the two-way flow valve 9 to have communication between (C) - (C). Thus, in step S514, the syringe pump a may start to draw pure water into the liquid storage ring 8A, while the syringe pump B starts to push the disinfectant to the detection chamber 4 to continue the disinfecting work. When the step S515 judges that the injection pump B finishes the disinfectant sample injection work and the injection pump A finishes the purified water extraction, the two-way flow valve 9 is switched to be communicated with the C-third and the (first) second in the step S516 without changing the liquid path of the multi-channel rotary valve 10. Subsequently, step S517 is executed, the injection pump B starts to pump purified water into the liquid storage ring 8B, and the injection pump a pushes the purified water to the detection chamber 4, so as to flush the detection chamber 4 and the liquid path. After the injection pump a finishes pushing and the injection pump B finishes extracting the purified water in step S518, the two-way flow valve 9 is switched to be communicated with the first two C and the second two C, and the multi-channel rotary valve 10 is switched to have the inlet of the liquid channel communicated with the air interface 54 in step S519. Thus, in step S520, the syringe pump a may start to draw air into the liquid storage ring 8A, and the syringe pump B starts to push purified water to the detection chamber 4, and the flushing operation is continued. Subsequently, after the step S521 judges that the syringe pump B finishes pushing the purified water, the syringe pump a starts to push air into the detection chamber by controlling the two-way flow valve 9 to be switched to the communication of C-C and (r) -C in the step S522, and the detection chamber 4 and the liquid path are emptied of the residual liquid. At this point, syringe pump B begins to draw air into reservoir ring B. After the step S523 judges that the syringe pump a has completed the liquid channel emptying step and the syringe pump B has exhausted air, the step S524 is executed to switch the two-way flow valve 9 to the communication of the first and second communication, and the syringe pump B is controlled to start pushing air to the detection chamber 4 in the step S525 to continue the liquid channel emptying operation. After judging that the syringe pump B completes the air pushing in step S526, the entire cleaning operation is finished.
Alternatively, in the judgment step performed by the control unit 1 described above, instead of making the judgment as to whether the certain operation is completed, the next step may be performed after a set fixed time interval has elapsed. The fixed time interval is more than or equal to the time required by the injection pump to finish one-time sample injection.
In the above-described cleaning and sterilizing operation, the switching of the two-way flow valve 9 is selectively suspended to complete the cleaning and sterilizing continuous operation using only the flow path of one syringe pump. Or the action time of the cleaning agent and the disinfectant is given by matching with the pause of the injection pump, which is beneficial to improving the cleaning and disinfecting effect. When cleaning, disinfecting and flushing are carried out, the same syringe pump can repeatedly carry out the same operation, namely, the syringe pump repeatedly carries out push-pull operation and cleaning, disinfecting or flushing in a reciprocating way, and the repeated operation can also enhance the cleaning effect.
The above cleaning processes using cleaning agent, disinfectant, purified water and air are only exemplary, and the corresponding cleaning agent can be reduced or increased according to the requirement, and only the corresponding cleaning unit interface needs to be reduced or increased correspondingly. Alternatively, when the number of fluid outlets of the multi-channel rotary valve 10 is not sufficient, two or more sub-ports may be integrated into a port corresponding to a certain fluid outlet of the multi-channel rotary valve by using additional three-way valves, for example, the first end and the second end of the three-way valve are respectively used as the outlet ports of the sub-ports, and the third end is used as the port corresponding to a certain fluid outlet of the multi-channel rotary valve. Further, a switch which can be automatically controlled or manually controlled can be arranged at the outlet end of one of the sub-interfaces of the three-way valve. By controlling both the switch and the multi-channel rotary valve 10, the fluid inlet of the multi-channel rotary valve 10 can be communicated with different sub-interfaces. Specifically, for example, in the above embodiment, the air interface and the purified water interface may be integrated into one air purified water interface 54, as shown in fig. 5 of the specification, the interface 54 is then divided into two paths by, for example, a three-way valve 551, to form two additional interfaces 5511 and 5512, which correspond to the external purified water bottle and the external air, respectively, and then a switch 552 may be separately provided on the interface to control the connection or disconnection of the interfaces. Since the cleaning process includes two successive operations of flushing with pure water and blowing with air, a normally closed switch may be selectively provided at a later interface, for example, the interface 5512 corresponding to the outside air. The control flow of the sample injection system can be the same as the previous embodiment until the syringe pump a pushes pure water to the detection chamber 4. However, in this alternative, after the syringe pump a completes the flushing operation to the detection chamber 4, the multi-channel rotary valve 10 may not switch the fluid path, and the fluid path inlet may be connected to the fluid path outlet of the corresponding port 54. It is necessary to open a normally closed switch located on the port 5512 corresponding to the outside air. After the switch is turned on, the injection pump A is controlled to start working, and air is pumped into the injector A. Similarly, when the syringe pump B finishes the operation of flushing the detection chamber 4, the multi-channel rotary valve 10 may finish the operation of sucking air into the syringe B without switching the fluid path. Alternatively, the switch may be a switch that can be opened by manual operation, or a switch whose opening and closing are controlled by the control unit 1. The above example is to integrate the air interface and the purified water interface, and those skilled in the art can also easily think that another two or more interfaces can also be integrated, and the operations corresponding to the other interfaces can be sequentially connected during execution or not connected in time, but no matter how modified, the operation of the sample injection system can be realized by additionally matching with a corresponding switch and changing the control flow similar to the above example. Therefore, on one hand, the multi-channel rotary valve can complete more required functions without selecting valves with more liquid path outlets, which is beneficial to controlling the cost of the whole system, and on the other hand, the multi-channel rotary valve with fixed liquid path outlets can be simply modified to complete the expansion of more functions. The above solution for expanding the liquid path outlets is only one of the embodiments, and alternatively, the multi-channel rotary valve 10 with the number of the liquid path outlets matching the required number may be directly selected.
In this embodiment there is also provided a bubble removal unit 6 for monitoring in real time whether the detection zone has bubbles present and retained which would have an effect on the detection of the sample. The bubble removing unit 6 is mainly composed of a water pumping unit 61 and a monitoring unit 62, and is matched with an opening arranged at one end of the detection chamber 4. The water pumping unit 61 communicates with an opening at one end of the detection chamber 4, and functions to push the liquid from the opening at one end of the detection chamber 4 toward the detection chamber 4, thereby pushing away the air bubbles staying in the detection chamber 4. The monitoring unit 62 is composed of an image acquisition unit and a display unit, and is controlled by the control unit 1 or a separate control unit. Image acquisition may use a small camera focused on the detection window of the detection area. Whether bubbles appear and are detained in the detection area is monitored in real time through the camera to judge whether influence sample detection. When the bubble is detained in the detection zone and influences the sample and detect, monitoring unit 62 can feedback control unit 1, and control unit 1 will send the instruction to pumping unit 61 to the liquid that can push away the bubble from the bottom of detection chamber 4 to the propelling movement in the detection chamber.
The water pumping unit 61 can utilize a pump valve in the sample injection system to provide power, and as shown in fig. 2 in the specification, a Y-shaped flow path valve 611 with three interfaces is used. The interface of the two-way flow valve 9 is connected to the first interface of the Y-shaped flow valve 611, and the normally pushed liquid sample is delivered to the detection chamber 4 through the second interface of the Y-shaped flow valve 611. The first and second ports of the Y-shaped flow path valve 611 constitute a main flow path of the Y-shaped flow path valve 611, which is a flow path used by the Y-shaped flow path valve at times other than when the bubble removal operation is performed. One end (bottom end in the figure) of the detection chamber 4 is further provided with, for example, a pinhole-type opening, and the third port of the Y-shaped channel valve 611 is connected to the opening to constitute a bubble removal channel. When the injection pump a or B pushes the liquid sample to the detection chamber 4, if the monitoring unit 62 monitors bubbles affecting the detection of the apparatus, the control unit 1 sends an instruction to the Y-shaped flow valve 611, the Y-shaped flow valve 611 is switched to be communicated with the bubble removing passage, and the liquid sample continuously pushed by the injection pump a or B after switching is injected through the bubble removing passage, that is, injected from the opening at the bottom of the detection chamber 4, so that the retained bubbles can be pushed away from bottom to top. When the monitoring unit 62 detects that the bubbles are removed, the Y-shaped flow valve 611 can receive the instruction from the control unit 1, and then switch to the situation of using the main flow path to continue the normal sample injection operation.
The provision of a single opening at one end of the detection chamber 4 for bubble removal facilitates the diversification of the bubble removal scheme. For example, in the detection of a liquid sample in a laboratory, the bubble removal may be performed by using the liquid sample or may be performed by using other liquid such as purified water other than the sample, depending on the specific condition of the sample. If purified water and other liquids are used, when one injection pump is used for sample injection, the other injection pump can connect the liquid path thereof with a required liquid interface through the multi-channel rotary valve 10, and the liquid is pumped into the injection pump to prepare for bubble removal.
Although the bubble removal process is implemented by pushing the sample from one end of the detection chamber 4, the sample in the detection chamber 4 may be pumped by a syringe pump to move the bubbles, and the bubble removal function may also be achieved. For example, when judging that there is the bubble, the syringe pump in the current work suspend work, carry out the back pumping operation of above-mentioned sample, back pumping operation can be once, also can be for carrying out repeatedly many times, judges simultaneously whether the bubble removes, if the bubble does not influence the accuracy that detects any more, then back pumping operation can stop, and the bubble of removing can not influence the detection again, and follow-up normal appearance that resumes.
In the above embodiment, two syringe pumps are used, but the system is not limited thereto. The number of syringe pump units is not limited to two, but may be more than three, four or five, etc., depending on the actual requirements. By selecting a suitable multi-way rotary valve and setting of the corresponding control unit 1, the cooperative and alternate work of a plurality of injection pumps can be realized. For a specific control flow, a person skilled in the art can easily expand the control flow of the two syringe pumps in the embodiment to complete continuous sampling, cleaning and bubble removal of the system.
It should be noted that the embodiments and features of the embodiments may be combined with each other without conflict. The design according to the invention can also be modified and finished in detail in order to improve various properties of the imaging system, which should also be regarded as a scope of protection of the invention.
While only certain embodiments of the present invention have been illustrated and described, it will be appreciated by those skilled in the art that changes may be made in this embodiment without departing from the principles and spirit of the invention, the scope of which is defined in the claims and their equivalents.