An automated liquid-liquid extraction fractionation method, apparatus, device, and medium

Abstract

The application discloses an automatic liquid-liquid extraction layer separation method, device, equipment and medium, and the method comprises the following steps: collecting the light intensity signal obtained by the photoelectric detection unit acting on the fluid in the liquid discharge pipeline based on the preset light path mode in real time at a preset frequency; calculating the real-time amplitude of the light intensity signal and the real-time amplitude variation degree in the preset window range; automatically identifying the current fluid state relative to the photoelectric detection unit in the liquid discharge pipeline according to the variation degree type, wherein the current fluid state comprises a pure liquid phase, an emulsion layer and a phase change interface; automatically controlling the opening and closing action of the electrically controlled switch device arranged on the liquid discharge pipeline and located downstream of the photoelectric detection unit according to the identified current fluid state, and realizing liquid-liquid extraction layer separation. The layer separation has high sensitivity and wide applicability, strong anti-interference ability, solves the problem of distinguishing in the same refractive index, is low in cost, accurate in distinguishing, and fast in response.

Description

Technical Field

[0001] This application relates to the field of analytical testing technology, and in particular, to an automated liquid-liquid extraction and separation method, apparatus, equipment, and medium. Background Technology

[0002] Liquid-liquid extraction (LLE), a classic sample pretreatment technique, is widely used in environmental monitoring (such as water quality, petroleum hydrocarbons, and volatile phenols), food safety (such as pesticide residue analysis), biomedicine, and petrochemicals. This process utilizes the difference in solubility or partition coefficients of the analyte in two immiscible solvents (usually an aqueous phase and an organic phase) to transfer the analyte from the matrix to the extractant, achieving separation through physical stratification.

[0003] Currently, the mainstream automated stratification / liquid level detection technologies in liquid-liquid extraction mainly include: (1) Capacitance / Conductivity Probing Method: The method of determining the liquid level by utilizing the sudden change in capacitance or conductivity when a probe contacts the liquid is only applicable to conductive liquids (such as aqueous phases). For "organic phase-to-organic phase" extraction, or when the organic phase is in the lower layer, the interface cannot be detected, and some probes may contaminate the organic solvent or interfere with subsequent tests.

[0004] (2) Vision-based visual recognition method: Using industrial cameras to capture images of the separatory funnel and then employing image processing algorithms to locate the phase interface is a costly method that is highly sensitive to lighting conditions. Furthermore, image recognition is prone to errors when the liquids are similar in color (e.g., both are transparent) or when droplets adhere to the walls.

[0005] (3) Ordinary photoelectric switch method: This method uses the difference in refraction of light at the gas-liquid interface to determine whether liquid is flowing through it. Limitations: It can usually only distinguish between "liquid presence" and "no liquid (air)". For two liquids that are both transparent and have similar refractive indices, the signal change is weak, making accurate phase separation impossible.

[0006] It is evident that automated pretreatment equipment faces the following core technical challenges in liquid-liquid separation: (1) Interface blurring and emulsion layer interference cannot be accurately identified: When processing complex samples (such as environmental sewage and biological samples), emulsion layers of varying thickness are often formed between the aqueous phase and the organic phase. Traditional sensors have difficulty defining their boundaries, resulting in impure separation or sample loss.

[0007] (2) Difficulty in distinguishing media with similar refractive indices: When the refractive indices of two liquids are very close (for example, the difference between some organic solvents and water is very small), or due to ambient light interference, conventional optical sensors cannot generate sufficient signal difference, making it difficult to distinguish and leading to misjudgment.

[0008] (3) Detection blind zone of non-conductive media: Traditional capacitive / conductive liquid level detection can only identify conductive water phase, but cannot distinguish between two non-conductive organic phases, or can not effectively monitor when organic phase flows out.

[0009] (4) Response lag: Image processing requires computation time and is usually combined with a peristaltic pump, making it difficult to achieve millisecond-level fluid flow cutoff. Summary of the Invention

[0010] This application provides an automated liquid-liquid extraction and layer separation method, which solves the technical problems of existing layer separation methods, such as high cost, inability to achieve accurate phase separation, susceptibility to errors, and slow response.

[0011] This application is achieved through the following solution: An automated liquid-liquid extraction and separation method includes the following steps: The photoelectric detection unit collects the light intensity signal obtained by the fluid in the drain pipe in real time according to the preset frequency and the preset optical path method. Calculate the real-time amplitude of the light intensity signal and the degree of real-time amplitude change within a preset window range; The current fluid state at the relative photoelectric detection unit in the drain pipe is automatically identified according to the type of change, wherein the current fluid state includes pure liquid phase, emulsion layer and phase change interface; The system automatically controls the opening and closing of an electronically controlled switch located downstream of the photoelectric detection unit on the drain pipe based on the identified current fluid state, thereby achieving liquid-liquid extraction and stratification separation.

[0012] Furthermore, before acquiring the light intensity signal obtained by the photoelectric detection unit acting on the fluid in the drainage pipe in real time at a preset frequency according to a preset optical path method, the process also includes the following steps: When the fluids in the drain pipe are air and a preset fluid, the light intensity signals of the photoelectric detection unit acting on the fluids in the drain pipe through the preset optical path are collected as the air reference value and the first phase reference value, respectively. The system determines whether the light source and detector are functioning properly based on the air reference value and the first phase reference value, and dynamically adjusts the light source current or the detector response intensity according to the detector's optimal monitoring range.

[0013] Furthermore, the photoelectric detection unit is installed outside the drain pipe and includes an emitting end and a receiving end connected to a light source. The light source includes visible light, infrared light, composite light, and ultraviolet light, and the optical path is either transmissive or total internal reflection.

[0014] Furthermore, the calculation of the real-time amplitude of the light intensity signal and the degree of real-time amplitude change within a preset window range specifically includes the following steps: The collected light intensity signals are processed in real time to calculate the real-time amplitude of the light intensity signal at each sampling point. Calculate the mean value of the current amplitude of the real-time amplitude sequence of the light intensity signal within the current time window of a preset length K; The rate of change of amplitude is calculated based on the absolute value of the difference between the current average amplitude and the average amplitude before the preset length K. The amplitude volatility is obtained by calculating the variance, standard deviation, first derivative, or frequency domain analysis value of the real-time amplitude during the drainage process.

[0015] Furthermore, before performing real-time processing on the collected light intensity signals and calculating the real-time amplitude of the light intensity signal at each sampling point, the following steps are also included: Turn on the electronic control switch and hold it for a set time. When the fluid flow rate in the drain pipe stabilizes, continuously collect the real-time amplitude of N data points to calculate the average value and obtain the reference value. The fluid in the drain pipe is determined according to the target fluid to be separated and retained, which is either the lower layer liquid or the supernatant liquid.

[0016] Furthermore, the current fluid state at the relative photoelectric detection unit within the drainage pipeline is automatically identified based on the type of change, specifically including the following steps: When the amplitude change rate is greater than the preset abrupt change threshold, or when the absolute value of the difference between the current average amplitude and the reference value is greater than the preset absolute threshold, the current fluid state at the relative photoelectric detection unit in the drain pipe is identified as a phase change interface. When the amplitude fluctuation rate is less than the preset stability threshold, the current fluid state at the relative photoelectric detection unit in the drain pipe is identified as pure liquid phase. When the amplitude fluctuation rate is greater than the preset noise threshold, the current fluid state at the relative photoelectric detection unit in the drain pipe is identified as emulsion layer.

[0017] Furthermore, the automatic control of the opening and closing of the electrically controlled switch device, located downstream of the photoelectric detection unit and installed on the drain pipe, based on the identified current fluid state, to achieve liquid-liquid extraction and stratification separation, specifically includes the following steps: When the electronic control switch is turned on to separate the lower layer liquid, if the current fluid state at the relative photoelectric detection unit in the drain pipe is identified as an emulsion layer or a phase change interface, the electronic control switch is turned off. When retaining the supernatant, turn on the electronic control switch. After draining the lower layer and emulsion, turn off the electronic control switch. The draining of the emulsion is determined based on whether the amplitude fluctuation rate recovers to less than the preset stable threshold.

[0018] Furthermore, when shutting down the electronically controlled switch, the following steps are also included: When a signal to shut down the electronically controlled switch is received, the injection pump or high-precision peristaltic pump connected to the electronically controlled switch is controlled to extract a fixed volume of fluid from the upper inner cavity of the electronically controlled switch and discharge it.

[0019] Furthermore, when shutting down the electronically controlled switch, the following steps are also included: When a signal to close the electronically controlled switch is received, the electronically controlled switch is closed after a set delay, allowing a fixed volume of fluid to be discharged from the upper cavity of the electronically controlled switch.

[0020] Furthermore, when the electronically controlled switch is turned off after a set delay, the set delay is statically set in advance based on the known density value of the discharged fluid.

[0021] Furthermore, when the electronically controlled switch is turned off after a set delay, the set delay is dynamically determined by looking up a table based on the real-time detection value of the density of the discharged fluid.

[0022] Furthermore, the electrically controlled switching device includes a solenoid valve, a high-precision peristaltic pump, an electric switching valve, and an electric clamping valve.

[0023] This application also provides an automated liquid-liquid extraction and separation apparatus, comprising: The light intensity signal acquisition module is used to acquire the light intensity signal obtained by the photoelectric detection unit acting on the fluid in the drain pipe in real time at a preset frequency according to a preset optical path. The fluctuation degree calculation module is used to calculate the real-time amplitude of the light intensity signal and the degree of real-time amplitude change within a preset window range; A fluid state recognition module is used to automatically identify the current fluid state at the relative photoelectric detection unit in the drain pipe according to the type of change, wherein the current fluid state includes pure liquid phase, emulsion layer and phase change interface; The switch control module is used to automatically control the opening and closing of the electronically controlled switch device located on the drain pipe and downstream of the photoelectric detection unit according to the identified current fluid state, so as to realize the liquid-liquid extraction and stratification separation.

[0024] This application also provides an electronic device comprising: a memory, a processor, and a computer program stored in the memory and executable on the processor, wherein the processor executes the computer program to implement the automated liquid-liquid extraction and separation method.

[0025] This application also provides a computer-readable storage medium having a computer program stored thereon, which, when executed by a processor, implements the automated liquid-liquid extraction and separation method.

[0026] This application also provides a computer program product, including a computer program or computer-executable instructions, which, when executed by a processor, implement the automated liquid-liquid extraction and separation method.

[0027] Compared with the prior art, this application can produce the following beneficial effects: This application has high sensitivity and wide applicability: compared with the conductivity method, this application does not depend on conductivity and can be applied to the separation of water from all organic solvents such as n-hexane, dichloromethane, and ethyl acetate; This application has strong anti-interference capabilities (solving interface ambiguity): by introducing real-time amplitude change within a preset window range to analyze and identify whether the current fluid state is a pure liquid phase, an emulsion layer, or a phase change interface, it can distinguish the chaotic signals generated by the emulsion layer (scattering chaotic region) from bubbles and electronic noise, preventing accidental or missed cutting at the emulsion layer. This application solves the problem of difficulty in accurately separating different liquid media with similar refractive indices: it adopts a transmission-type (detecting absorbance differences) or total internal reflection-type (detecting refractive index differences) optical path method, thereby utilizing the absorbance differences or total internal reflection characteristics of different liquid media (such as water phase / organic phase) at specific wavelengths (such as near-infrared), rather than simply the physical refraction angle, so that even if the two phases appear to be transparent and have similar refractive indices, they can be accurately distinguished by spectral absorption characteristics.

[0028] This application achieves high-precision separation processing at low cost: it eliminates the need for expensive industrial cameras and image processing computers, and can achieve millisecond-level response using only low-cost photoelectric detection units such as photodiodes and MCUs. It not only has a fast response speed but also low hardware requirements and low cost.

[0029] In addition to the purposes, features, and advantages described above, this application has other purposes, features, and advantages. A further detailed description of this application will be provided below with reference to the figures. Attached Figure Description

[0030] The accompanying drawings, which are incorporated in and form part of this specification, illustrate embodiments consistent with this application and, together with the description, serve to explain the principles of this application.

[0031] To more clearly illustrate the technical solutions in the embodiments of this application or the prior art, the drawings used in the description of the embodiments or the prior art will be briefly introduced below. Obviously, for those skilled in the art, other drawings can be obtained based on these drawings without creative effort, wherein: Figure 1 This is a schematic diagram of the automated liquid-liquid extraction and separation device of this application. Figure 2 This is a schematic flowchart of an automated liquid-liquid extraction and separation method according to a preferred embodiment of this application; Figure 3 This is a schematic flowchart of an automated liquid-liquid extraction and separation method according to another preferred embodiment of this application; Figure 4 This is a schematic diagram of the light intensity amplitude variation curve of benzene separated from the organic phase in the aqueous phase according to a preferred embodiment of this application; Figure 5 This is a schematic diagram of the modules of the automated liquid-liquid extraction and separation device according to a preferred embodiment of this application; Figure 6 This is a schematic block diagram of an electronic device according to a preferred embodiment of this application; Figure 7 This is a schematic diagram of the internal structure of a computer device according to a preferred embodiment of this application.

[0032] In the diagram: 1. Separation container; 2. Microcontroller; 3. Light source; 4. Transmitter; 5. Drainage pipeline; 6. Electrical control switch; 7. Receiver. Detailed Implementation

[0033] To better understand the technical solution of this application, a detailed description will be provided below in conjunction with the accompanying drawings and specific implementation methods.

[0034] It should be noted that the executing entity in this embodiment can be a computing service system with data processing, network communication, and program execution functions, such as a tablet computer, personal computer, or mobile phone, or an automated liquid-liquid extraction and separation device capable of performing the above functions. The automated liquid-liquid extraction and separation device mainly consists of four parts: a fluid pipeline assembly, a photoelectric detection unit, an execution control unit, and an algorithm processing center (see...). Figure 1 ).

[0035] 1. Hardware Structure Description The fluid piping assembly includes a separation container 1 and a drain pipe 5. The bottom of the separation container 1 is connected to the drain pipe 5, which is made of a transparent material (such as Teflon or quartz) and has a diameter of 1mm-3mm.

[0036] Photoelectric detection unit: installed on the outside of the drain pipe, including light source 3, transmitter 4 and receiver 7.

[0037] The light source 3 can be an LED light source (such as a visible light or infrared light LED light source). The receiver 7 includes a detector.

[0038] Specifically, visible light is used for organic layers that change color, while infrared light is used for organic layers that do not change color. This utilizes the strong absorption of OH bonds in water molecules in the near-infrared region, while most organic solvents (CH bonds) have weak absorption in this wavelength range. In practical applications, composite light sources can also be used to cover both visible and infrared wavelengths.

[0039] Optical path design: Transmission type (detecting absorbance difference) or total internal reflection type (TIR, detecting refractive index difference) is adopted. When an aqueous phase flows through the tube, near-infrared (or visible light) is strongly absorbed, resulting in a lower voltage detected by the receiver; when an organic phase flows through the tube, the light transmittance is high, and the voltage detected by the receiver is relatively higher.

[0040] Execution control unit: The electrically controlled switching device 6 (such as a solenoid valve or an electric clamp valve) is located downstream of the photoelectric detection unit. The required response time is <20ms.

[0041] Microcontroller 2 (MCU): Connected to the photoelectric detection unit and the electronic control switch device 6 respectively, and executes high-frequency sampling and control algorithms.

[0042] The following description uses an automated liquid-liquid extraction and separation equipment as an example to illustrate this embodiment and the following embodiments.

[0043] like Figure 2 As shown, to address the aforementioned technical problems, a preferred embodiment of this application provides an automated liquid-liquid extraction and separation method, comprising the following steps: S1. Real-time acquisition of light intensity signals obtained by the photoelectric detection unit acting on the fluid in the drain pipe through a transmission (detecting absorbance difference) or total internal reflection (detecting refractive index difference) optical path at a preset frequency (e.g., 500Hz). S2. Calculate the real-time amplitude of the light intensity signal and the degree of real-time amplitude change within a preset window range; S3. Automatically identify the current fluid state at the relative photoelectric detection unit in the drain pipe according to the type of change, wherein the current fluid state includes pure liquid phase, emulsion layer and phase change interface; S4. Based on the identified current fluid state, automatically control the opening and closing of the electronically controlled switch device located on the drain pipe and downstream of the photoelectric detection unit to achieve liquid-liquid extraction and stratification separation.

[0044] Compared with the prior art, this application can produce the following beneficial effects: This embodiment features high sensitivity and wide applicability: compared to the conductivity method, this application does not depend on conductivity and can be applied to the separation of all organic solvents such as n-hexane, dichloromethane, and ethyl acetate from water; This embodiment has strong anti-interference capabilities (solving interface ambiguity): by introducing real-time amplitude change analysis within a preset window range, it can identify whether the current fluid state is a pure liquid phase, an emulsion layer, or a phase change interface. It can distinguish the chaotic signals generated by the emulsion layer (scattering chaotic region) from bubbles and electronic noise, preventing accidental or missed cutting at the emulsion layer. This embodiment solves the problem of difficult precise separation of different liquid media with similar refractive indices: it adopts a transmission-type (detecting absorbance differences) or total internal reflection-type (detecting refractive index differences) optical path method, thereby utilizing the absorbance differences or total internal reflection characteristics of different liquid media (such as water phase / organic phase) at specific wavelengths (such as near-infrared), rather than simply the physical refraction angle, so that even if the two phases appear to be transparent and have similar refractive indices, they can be accurately distinguished through spectral characteristics.

[0045] This embodiment achieves high-precision separation processing at low cost: it does not require expensive industrial cameras and image processing computers, but only low-cost photoelectric detection units such as photodiodes and MCUs can achieve millisecond-level response. It not only has a fast response speed, but also low hardware requirements and low cost.

[0046] like Figure 3 As shown, in a preferred embodiment of this application, before acquiring the light intensity signal obtained by the photoelectric detection unit acting on the fluid in the drain pipe through a transmission (detecting absorbance difference) or total internal reflection (detecting refractive index difference) optical path at a preset frequency in real time, the method further includes the following steps: S0. When the fluids in the drain pipe are air and a preset fluid, the light intensity signals of the photoelectric detection unit acting on the fluids in the drain pipe are collected as the air reference value and the first phase reference value, respectively. The system determines whether the light source and detector are functioning properly based on the air reference value and the first phase reference value, and dynamically adjusts the light source current or the detector response intensity according to the detector's optimal monitoring range.

[0047] In this embodiment, before the equipment operates, when the fluids in the drain pipe are air and a preset fluid, the light intensity signals of the photoelectric detection unit acting on the fluids in the drain pipe are collected as the air reference value and the first phase reference value. The reading of these two reference values ​​is mainly used for the normality test of the equipment before use. By judging whether the light intensity signal is within the normal range, the accuracy and reliability of subsequent identification and calculation are ensured. This is because the equipment can only enter the formal operation process when the light intensity signal falls within the normal response range of the detector. Otherwise, it is necessary to adjust the relevant parts of the equipment, such as replacing or adjusting the parameters of the photoelectric detection unit, replacing the drain pipe with a different transparency, etc., to ultimately ensure that the subsequent automated layer separation operation can operate normally and reliably.

[0048] In a preferred embodiment of this application, the photoelectric detection unit is installed outside the drain pipe and includes an emitting end and a receiving end connected to a light source, wherein the light source includes visible light, infrared light, composite light source, and ultraviolet light.

[0049] In this embodiment, the light source can be selected as an LED light source (such as a visible light or infrared light LED light source) as needed. Visible light is used for organic layers that undergo color changes, while infrared light is used for organic layers that do not undergo color changes. This utilizes the strong absorption characteristics of the OH bonds in water molecules in the near-infrared region, while most organic solvents (CH bonds) have weak absorption in this wavelength range. Besides visible and infrared light, ultraviolet LED light sources can be used for solvents with strong UV absorption due to conjugated double bonds. Therefore, by selecting a suitable light source, accurate detection of different types of solutions can be achieved, offering wide adaptability, flexibility, reliability, and low cost.

[0050] In a preferred embodiment of this application, the calculation of the real-time amplitude of the light intensity signal and the degree of change of the real-time amplitude within a preset window range (e.g., a 50ms window) specifically includes the following steps: S21. Process the collected light intensity signals in real time and calculate the real-time amplitude of the light intensity signal at each sampling point (the most recent N sampling points); S22. During the drainage process, first calculate the current average amplitude of the real-time amplitude series of the light intensity signal within the current time window of a preset length K (e.g., 50). It is used to determine the overall change in the transmittance of a liquid; S23. Based on the current average amplitude and the average amplitude before the preset length K. The absolute value of the difference is used to calculate the rate of change of amplitude: ; S24. Calculate the variance, standard deviation, first derivative, or frequency domain analysis value of the real-time amplitude during the drainage process to obtain the amplitude volatility: ; in,V i It represents the real-time amplitude of all obtained sampling points.

[0051] In this embodiment, when calculating the real-time amplitude of the light intensity signal and the degree of real-time amplitude change within a preset window range, the current average amplitude of a data column of length K (e.g., 50) is first obtained. This is used to determine the overall change in the transmittance of the liquid, and then based on the current average amplitude... The amplitude change rate is calculated to capture amplitude "abrupt changes." These "abrupt changes" are used to accurately capture the instant of phase transition when "the first liquid is emptied and the second liquid has just arrived," i.e., the phase transition interface. Simultaneously, the amplitude fluctuation rate is calculated using the variance or standard deviation of the liquid discharge process data to identify the emulsion layer. Due to the scattering effect of the emulsion droplets on light, the signal amplitude fluctuates drastically. Therefore, the amplitude fluctuation rate can be an effective indicator for accurately identifying the emulsion layer. In other words, this embodiment utilizes the amplitude change rate and amplitude fluctuation rate as core indicators for identifying the emulsion layer, phase transition interface, and pure liquid phase, based on the characteristics of the emulsion layer, phase transition interface, and pure liquid phase itself. This accurately solves the identification problem of interface ambiguity and similar refractive indices of different liquid media, thereby achieving precise separation of automated liquid-liquid extraction layers.

[0052] In a preferred embodiment of this application, before performing real-time processing on the acquired light intensity signal and calculating the real-time amplitude of the light intensity signal at each sampling point, the following steps are also included: S20. Turn on the electronic control switch and hold it for a set time (e.g., 200ms). Wait for the fluid flow rate in the drain pipe to stabilize, flush away any air bubbles that may be present at the pipe opening, and then continuously collect samples. N The baseline value is obtained by calculating the average real-time amplitude of 50 data points: ; The fluid in the drainage pipeline is determined according to the target fluid to be separated and retained, and is either a known lower layer liquid or a supernatant liquid.

[0053] In this embodiment, the collected light intensity signals are processed in real time. Before calculating the real-time amplitude of the light intensity signal at each sampling point, the electronic control switch is activated and held for a set time (e.g., 200ms) to wait for the fluid flow rate in the drain pipe to stabilize. After flushing away any air bubbles that may be present at the pipe opening, continuous sampling is then performed. N The average real-time amplitude of each data point (e.g., 50) is used to obtain a baseline value. The purpose is to ensure the accuracy and reliability of the stratification separation operation based on different solvents and detector cells with different transmittances, so as to adapt to different colored solvents and detector cells with different transmittances. The baseline must be recalibrated before each separation, instead of using a fixed threshold that may fail due to environmental changes.

[0054] In a preferred embodiment of this application, the current fluid state relative to the photoelectric detection unit within the drainage pipeline is automatically identified based on the type of change, specifically including the following steps: S31. When the amplitude change rate is greater than the preset abrupt change threshold, or when the absolute value of the difference between the current average amplitude and the reference value is greater than the preset absolute threshold, the current fluid state at the relative photoelectric detection unit in the drain pipe is identified as a phase change interface. S32. When the amplitude fluctuation rate is less than the preset stability threshold, the current fluid state at the relative photoelectric detection unit in the drain pipe is identified as pure liquid phase. When the amplitude fluctuation rate is greater than the preset noise threshold (e.g., if the amplitude fluctuation rate exceeds the signal value of the noise threshold by N times, generally set to 2~5, the solenoid valve is immediately closed), the current fluid state at the relative photoelectric detection unit in the drain pipe is identified as emulsion layer.

[0055] In this embodiment, the current fluid state at the photoelectric detection unit relative to the drain pipe is automatically identified as a pure liquid phase, an emulsion layer, or a phase transition interface based on the amplitude change rate and amplitude fluctuation rate. If it is a pure liquid phase, the amplitude fluctuation rate is less than a preset stability threshold, resulting in stable signal amplitude and extremely low variance; therefore, the current fluid state at the photoelectric detection unit is automatically identified as a pure liquid phase. Due to the light scattering effect of the emulsion droplets in the emulsion layer, when the amplitude fluctuation rate exceeds a preset noise threshold, the signal amplitude fluctuates violently, and the variance increases significantly. If the amplitude fluctuation rate exceeds the preset noise threshold, the current fluid state at the photoelectric detection unit is automatically identified as an emulsion layer. Similarly, when the signal amplitude undergoes a step change (e.g., from high transmittance to low transmittance), the current fluid state at the photoelectric detection unit is automatically identified as a phase transition interface. Figure 4 As shown, taking the separation of organic phase benzene from aqueous phase and the detection of complexes in benzene as an example, in the stage from A0 to A, the signal amplitude is stable and the variance is small. Therefore, the system automatically identifies the current fluid state (pure liquid phase) relative to the photoelectric detection unit in the drain pipe. The inflection points include A, B, C, D, E, and F, where: The range A0 to A represents the signal value of the lower layer of liquid to be separated; the range A to C represents the signal fluctuations generated during liquid level exchange.

[0056] Under normal circumstances, when the two phases separate, the signal should go directly from A to C without generating point B. However, due to the effect of emulsification, a segment from B to C will appear, and the segment between the intersection of the extended line CD and AB corresponds to the start and end time of the emulsion layer.

[0057] CD represents the organic phase layer that remains for a period of time. Similarly, DEF represents the signal fluctuations during liquid level exchange.

[0058] If there is no emulsification, the signal curve should show the ACDF pattern. However, due to the emulsification that occurs between the organic and aqueous phases during the actual reaction, fluctuations in the BC and DE segments will occur on the signal curve during the separation process.

[0059] In a preferred embodiment of this application, the automatic control of the opening and closing of an electrically controlled switch device located downstream of the photoelectric detection unit on the drain pipe, based on the identified current fluid state, to achieve liquid-liquid extraction and stratification separation, specifically includes the following steps: S41. When the electronic control switch is turned on to separate the lower layer liquid, if the current fluid state at the relative photoelectric detection unit in the drain pipe is identified as an emulsion layer or a phase change interface, the electronic control switch is turned off. S42. When retaining the supernatant, turn on the electronic control switch device. After draining the lower layer liquid and emulsion layer, turn off the electronic control switch device. The draining of the emulsion layer is determined based on whether the amplitude fluctuation rate recovers to less than the preset stable threshold.

[0060] In this embodiment, after identifying the current fluid state, the microcontroller 2 will automatically send different action commands to the electronic control switch device based on whether the current fluid state is a pure liquid phase, an emulsion layer, or a phase change interface, and whether the current task is to separate the lower layer liquid or retain the supernatant. For example, when facing the task of separating the lower layer liquid, it is necessary to ensure the quality of the separated lower layer liquid and that there are no impurities. Therefore, when the current fluid state at the photoelectric detection unit in the drain pipe is identified as an emulsion layer or a phase change interface, the microcontroller 2 sends a command to immediately shut down the electronic control switch device to prevent the emulsion or supernatant from entering the separated lower layer liquid, thus achieving accurate separation of the lower layer liquid; while when When faced with the task of retaining the supernatant, it is necessary to ensure the quality of the supernatant remaining in the separation container 1 after separation, and to prevent emulsion or lower layer liquid from accumulating in the supernatant. At this time, the lower layer liquid is drained first, followed by the emulsion layer. At this time, the amplitude fluctuation rate will be greater than the preset noise threshold. After the emulsion layer is drained, the pure liquid phase supernatant flows out. At this time, the microcontroller 2 determines whether the emulsion layer has been drained based on whether the amplitude fluctuation rate has recovered to less than the preset stability threshold. Finally, it sends a command to immediately shut down the electronic control switch device to ensure that only the supernatant remains in the separation container 1, thus ensuring the sensitivity, reliability, stability and accuracy of the layer separation.

[0061] In a preferred embodiment of this application, when turning off the electronically controlled switch device, the step further includes: S401. When a signal to close the electronically controlled switch is received, the injection pump or high-precision peristaltic pump connected to the electronically controlled switch is controlled to extract a fixed volume of fluid from the upper inner cavity of the electronically controlled switch and discharge it.

[0062] Since the photoelectric detection unit and the electronic control switch cannot overlap, and the electronic control switch is generally located downstream of the photoelectric detection unit, after the microcontroller 2 completes the current fluid state based on the detection result of the photoelectric detection unit and sends a command to the electronic control switch to close it, there may still be a section of residual liquid in the upper inner cavity of the electronic control switch. Since the judgment principle is consistent, the volume of this residual liquid is consistent each time. Therefore, an injection pump or a high-precision peristaltic pump can be connected to the electronic control switch. After the electronic control switch receives the command to close, a fixed volume of residual solution can be extracted and discharged to obtain a completely separated sample.

[0063] In a preferred embodiment of this application, when turning off the electronically controlled switch device, the step further includes: S402. When a signal to close the electronically controlled switch is received, the electronically controlled switch is closed after a set delay, so that a fixed volume of fluid in the upper cavity of the electronically controlled switch is discharged.

[0064] Unlike the above embodiments, this embodiment, considering hardware costs, does not add an injection pump or a high-precision peristaltic pump. Instead, it controls the delayed shutdown of the electronic control switch to discharge a fixed volume of fluid from the upper inner cavity of the electronic control switch. That is, when the current fluid state is identified and a signal to shut down the electronic control switch is received, the electronic control switch is not shut down immediately, but is shut down after a set delay, allowing the solution to continue flowing through the electronic control switch for a period of time before being discharged. This ensures that a fixed volume of fluid in the upper inner cavity of the electronic control switch is discharged, avoiding the possibility of residual liquid remaining in the upper inner cavity of the electronic control switch, which could affect the separation quality of the layered solution.

[0065] In a preferred embodiment of this application, when the electronically controlled switch device is turned off after a set delay in step S402, the set delay is statically set in advance based on the known density value of the discharged fluid. Since the known density value of the discharged fluid is known in advance, the flow rate of the discharged fluid can be estimated. Based on the estimated flow rate, a static set delay can be set to ensure that a fixed volume of fluid in the upper cavity of the electronically controlled switch device can flow out within the static set delay.

[0066] In a preferred embodiment of this application, when the electronically controlled switch is turned off after a set delay in step S402, the set delay is dynamically determined by looking up a table based on the real-time density detection value of the discharged fluid.

[0067] When the solution density varies, the flow rate also varies. If the statically set time duration is uniformly used in the aforementioned embodiments to delay the closing of the electronic control switch, problems may arise such as insufficient or excessive time. This could lead to the fixed volume of fluid in the upper cavity of the electronic control switch not being drained in time or not being able to be stopped in time, resulting in the mixing of other solutions. Therefore, unlike the aforementioned embodiments where a static set time duration is artificially set to control the delayed closing of the electronic control switch, this embodiment dynamically determines the set time duration based on the real-time detection value of the density of the drained fluid, i.e., this embodiment... Based on the density of the discharged fluid, the corresponding set time can be dynamically determined by automatically looking up a table (a pre-stored density-flow rate correspondence table). The entire process requires no manual intervention, is highly automated and adaptable, and can automatically and dynamically adapt the set time delay to close the electronic control switch device according to the different flow rates of the current solution. This ensures that the current set time matches the current flow rate of the solution, allowing sufficient time for the fixed volume of fluid in the upper cavity of the electronic control switch device to be discharged in time and to be cut off in time to prevent the mixing of other solutions, thus ensuring the separation quality of the stratified solution.

[0068] In a preferred embodiment of this application, the electrically controlled switch device includes a solenoid valve, a high-precision peristaltic pump, an electric switching valve, and an electric clamp valve. This embodiment uses a solenoid valve, which has a universal structure, is easy to control, has a fast response, and is low in cost.

[0069] In the above embodiment, the following replacement method can be adopted: Total internal reflection (TIR) ​​probe: The photoelectric component is made into a cone-shaped probe and inserted directly into the liquid, rather than transmitting through the outside of the tube.

[0070] Capacitive-photoelectric dual-mode fusion: A capacitive sensor is connected in parallel with photoelectric detection, using the capacitive signal as the "absolute anchor point" of the aqueous phase, and the photoelectric signal as a fine means of distinguishing between the organic phase and the emulsion layer.

[0071] like Figure 5 As shown, another preferred embodiment of this application also provides an automated liquid-liquid extraction and separation apparatus, comprising: The light intensity signal acquisition module is used to acquire the light intensity signal obtained by the photoelectric detection unit acting on the fluid in the drain pipe in real time at a preset frequency according to a preset optical path. The fluctuation degree calculation module is used to calculate the real-time amplitude of the light intensity signal and the degree of real-time amplitude change within a preset window range; A fluid state recognition module is used to automatically identify the current fluid state at the relative photoelectric detection unit in the drain pipe according to the type of change, wherein the current fluid state includes pure liquid phase, emulsion layer and phase change interface; The switch control module is used to automatically control the opening and closing of the electronically controlled switch device located on the drain pipe and downstream of the photoelectric detection unit according to the identified current fluid state, so as to realize the liquid-liquid extraction and stratification separation.

[0072] The automated liquid-liquid extraction and separation device provided in this embodiment employs the automated liquid-liquid extraction and separation method described in the above embodiments, solving the technical problems of high cost, inability to achieve accurate phase separation, susceptibility to errors, and slow response in existing separation methods. Compared with the prior art, the beneficial effects of the automated liquid-liquid extraction and separation device provided in this embodiment are the same as those of the automated liquid-liquid extraction and separation method provided in the above embodiments, and other technical features in the automated liquid-liquid extraction and separation device are the same as those disclosed in the methods of the above embodiments, and will not be repeated here.

[0073] like Figure 6 As shown, a preferred embodiment of this embodiment also provides an electronic device, including a memory, a processor, and a computer program stored in the memory and executable on the processor. When the processor executes the computer program, it implements the steps of the automated liquid-liquid extraction and separation method described in the above embodiment.

[0074] This embodiment also provides an electronic device that uses the automated liquid-liquid extraction and layer separation method in the above embodiments to solve the technical problems of high cost, inability to achieve accurate phase separation, easy error, and slow response of existing layer separation methods. Compared with the prior art, the beneficial effects of the electronic device provided in this embodiment are the same as those of the automated liquid-liquid extraction and layer separation method provided in the above embodiments, and other technical features of the electronic device are the same as those disclosed in the methods of the above embodiments, which will not be repeated here.

[0075] like Figure 7 As shown, a preferred embodiment of this application also provides a computer device, which may be a terminal or a liveness detection server, and its internal structure diagram may be as follows. Figure 7 As shown, the computer device includes a processor, memory, and a network interface connected via a system bus. The processor provides computing and control capabilities. The memory includes a non-volatile storage medium and internal memory. The non-volatile storage medium stores the operating system and computer programs. The internal memory provides an environment for the operation of the operating system and computer programs in the non-volatile storage medium. The network interface is used to communicate with other external computer devices via a network connection. When the computer program is executed by the processor, it implements the steps of the aforementioned automated liquid-liquid extraction and separation method.

[0076] Those skilled in the art will understand that Figure 7The structure shown is merely a block diagram of a portion of the structure related to the solution of this embodiment, and does not constitute a limitation on the computer device to which the solution of this embodiment is applied. The specific computer device may include more or fewer components than shown in the figure, or combine certain components, or have different component arrangements.

[0077] The computer device provided in this embodiment adopts the automated liquid-liquid extraction and layer separation method in the above embodiment, which solves the technical problems of high cost, inability to achieve accurate phase separation, easy error and slow response of existing layer separation methods. Compared with the prior art, the beneficial effects of the computer device provided in this embodiment are the same as the beneficial effects of the automated liquid-liquid extraction and layer separation method provided in the above embodiment. In addition, other technical features in the electronic device are the same as the features disclosed in the method of the above embodiment, and will not be repeated here.

[0078] A preferred embodiment of this application also provides a storage medium, the storage medium including a stored program, which, when the program is executed, controls the device where the storage medium is located to perform the steps of the automated liquid-liquid extraction and separation method in the above embodiments.

[0079] In summary, this application, based on real-time photoelectric sensing combined with signal morphology analysis algorithms, utilizes the differences in absorbance or total internal reflection characteristics of different media (aqueous / organic phases) at specific wavelengths (such as near-infrared) to distinguish two phases through spectral characteristics even when their refractive indices are similar, thereby achieving the following objectives: (1) Fully enclosed automated operation: completely isolates people from toxic reagents and eliminates occupational health hazards.

[0080] (2) Closed pipeline system: Reduces the exposed area of ​​organic solvents and operating time, significantly reduces the loss of volatile components, and improves the recovery rate.

[0081] (3) Standardized machine operation: eliminate human visual errors and operator fatigue, and ensure consistency in the processing of large batches of samples.

[0082] (4) High-precision intelligent phase separation: Through photoelectric sensors and volatility algorithms, the problem of interface ambiguity and identification of liquids with the same refractive index is accurately solved.

[0083] It should be noted that the steps shown in the flowchart in the accompanying drawings can be executed in a computer system such as a set of computer-executable instructions, and although a logical order is shown in the flowchart, in some cases the steps shown or described may be executed in a different order than that shown here.

[0084] If the functions described in this embodiment are implemented as software functional units and sold or used as independent products, they can be stored in one or more computing device-readable storage media. Based on this understanding, the parts of this embodiment that contribute to the prior art or the technical solution can be embodied in the form of a software product. This software product is stored in a storage medium and includes several instructions to cause a computing device (which may be a personal computer, server, mobile computing device, or network device, etc.) to execute all or part of the steps of the methods described in the various embodiments of this embodiment. The aforementioned storage media include: USB flash drives, portable hard drives, read-only memory (ROM), random access memory (RAM), magnetic disks, optical disks, and other media capable of storing program code.

[0085] Those skilled in the art will understand that the embodiments of this example can be provided as methods, systems, or computer program products. Therefore, this example can take the form of a completely hardware embodiment, a completely software embodiment, or an embodiment combining software and hardware aspects. Furthermore, this example can take the form of a computer program product implemented on one or more computer-usable storage media (including but not limited to disk storage, CD-ROM, optical storage, etc.) that include computer-usable program code. The solutions in this example can be implemented using various computer languages, such as the object-oriented programming language C++ and the embedded programming language C.

[0086] This embodiment is described with reference to flowchart illustrations and / or block diagrams of the method, apparatus (system), and computer program product according to this embodiment. It should be understood that each block of the flowchart illustrations and / or block diagrams, and combinations of blocks in the flowchart illustrations and / or block diagrams, can be implemented by computer program instructions. These computer program instructions can be provided to a processor of a general-purpose computer, special-purpose computer, embedded processor, or other programmable data processing apparatus to produce a machine, such that the instructions, which execute via the processor of the computer or other programmable data processing apparatus, generate instructions for implementing the flowchart illustrations. Figure 1 One or more processes and / or boxes Figure 1 A system that specifies functions in one or more boxes.

[0087] These computer program instructions may also be stored in a computer-readable storage medium that can direct a computer or other programmable data processing device to function in a particular manner, such that the instructions stored in the computer-readable storage medium produce an article of manufacture including an instruction set implemented in a process. Figure 1 One or more processes and / or boxes Figure 1 The function specified in one or more boxes.

[0088] These computer program instructions may also be loaded onto a computer or other programmable data processing equipment to cause a series of operational steps to be performed on the computer or other programmable equipment to produce a computer-implemented process, thereby providing instructions that execute on the computer or other programmable equipment for implementing the process. Figure 1 One or more processes and / or boxes Figure 1 The steps of the function specified in one or more boxes.

[0089] This embodiment also provides a computer program product, including a computer program that, when executed by a processor, implements the steps of the automated liquid-liquid extraction and separation method described above.

[0090] The computer program product provided in this embodiment solves the technical problems of existing layer separation methods, such as high cost, inability to achieve accurate phase separation, susceptibility to errors, and slow response. Compared with the prior art, the beneficial effects of the computer program product provided in this embodiment are the same as those of the automated liquid-liquid extraction layer separation method provided in the above embodiments, and will not be repeated here.

[0091] Obviously, those skilled in the art can make various modifications and variations to this embodiment without departing from the spirit and scope of this embodiment. Therefore, if these modifications and variations of this embodiment fall within the scope of the claims of this embodiment and their equivalents, this embodiment is also intended to include these modifications and variations.

Claims

1. An automated liquid-liquid extraction and layer separation method, characterized in that, Including the following steps: The photoelectric detection unit collects the light intensity signal obtained by the fluid in the drain pipe in real time according to the preset frequency and the preset optical path method. Calculate the real-time amplitude of the light intensity signal and the degree of real-time amplitude change within a preset window range; The current fluid state at the relative photoelectric detection unit in the drain pipe is automatically identified according to the type of change, wherein the current fluid state includes pure liquid phase, emulsion layer and phase change interface; The system automatically controls the opening and closing of an electronically controlled switch located downstream of the photoelectric detection unit on the drain pipe based on the identified current fluid state, thereby achieving liquid-liquid extraction and stratification separation.

2. The automated liquid-liquid extraction and separation method according to claim 1, characterized in that, Before acquiring the light intensity signal obtained by the photoelectric detection unit acting on the fluid in the drainage pipe in real time at a preset frequency based on a preset optical path, the following steps are also included: When the fluids in the drain pipe are air and a preset fluid, the light intensity signals of the photoelectric detection unit acting on the fluids in the drain pipe based on the preset optical path are collected as the air reference value and the first phase reference value, respectively. The system determines whether the light source and detector are functioning properly based on the air reference value and the first phase reference value, and dynamically adjusts the light source current or the detector response intensity according to the detector's optimal monitoring range.

3. The automated liquid-liquid extraction and layer separation method according to claim 1, characterized in that, The photoelectric detection unit is installed on the outside of the drain pipe and includes an emitting end and a receiving end connected to a light source. The light source includes visible light, infrared light, composite light, and ultraviolet light.

4. The automated liquid-liquid extraction and layer separation method according to claim 1, characterized in that, The calculation of the real-time amplitude of the light intensity signal and the degree of real-time amplitude change within a preset window range specifically includes the following steps: The collected light intensity signals are processed in real time to calculate the real-time amplitude of the light intensity signal at each sampling point. Calculate the mean value of the current amplitude of the real-time amplitude sequence of the light intensity signal within the current time window of a preset length K; The rate of change of amplitude is calculated based on the absolute value of the difference between the current average amplitude and the average amplitude before the preset length K. The amplitude volatility is obtained by calculating the variance, standard deviation, first derivative, or frequency domain analysis value of the real-time amplitude during the drainage process.

5. The automated liquid-liquid extraction and separation method according to claim 4, characterized in that, Before performing real-time processing on the collected light intensity signals and calculating the real-time amplitude of the light intensity signal at each sampling point, the following steps are also included: Turn on the electronic control switch and hold it for a set time. When the fluid flow rate in the drain pipe stabilizes, continuously collect the real-time amplitude of N data points to calculate the average value and obtain the reference value. The fluid in the drain pipe is determined according to the target fluid to be separated and retained, which is either the lower layer liquid or the supernatant liquid.

6. The automated liquid-liquid extraction and separation method according to claim 5, characterized in that, The system automatically identifies the current fluid state relative to the photoelectric detection unit within the drainage pipeline based on the type of change, specifically including the following steps: When the amplitude change rate is greater than the preset abrupt change threshold, or when the absolute value of the difference between the current average amplitude and the reference value is greater than the preset absolute threshold, the current fluid state at the relative photoelectric detection unit in the drain pipe is identified as a phase change interface. When the amplitude fluctuation rate is less than the preset stability threshold, the current fluid state at the relative photoelectric detection unit in the drain pipe is identified as pure liquid phase. When the amplitude fluctuation rate is greater than the preset noise threshold, the current fluid state at the relative photoelectric detection unit in the drain pipe is identified as emulsion layer.

7. The automated liquid-liquid extraction and layer separation method according to claim 6, characterized in that, The automatic control of the opening and closing of the electronically controlled switch device, located downstream of the photoelectric detection unit and installed on the drain pipe, based on the identified current fluid state, to achieve liquid-liquid extraction and stratification separation, specifically includes the following steps: When the electronic control switch is turned on to separate the lower layer liquid, if the current fluid state at the relative photoelectric detection unit in the drain pipe is identified as an emulsion layer or a phase change interface, the electronic control switch is turned off. When retaining the supernatant, turn on the electronic control switch. After draining the lower layer and emulsion, turn off the electronic control switch. The draining of the emulsion is determined based on whether the amplitude fluctuation rate recovers to less than the preset stable threshold.

8. The automated liquid-liquid extraction and layer separation method according to claim 7, characterized in that, When shutting down an electrically controlled switch, the following steps are also included: When a signal to shut down the electronically controlled switch is received, the injection pump or high-precision peristaltic pump connected to the electronically controlled switch is controlled to extract a fixed volume of fluid from the upper inner cavity of the electronically controlled switch and discharge it.

9. The automated liquid-liquid extraction and layer separation method according to claim 7, characterized in that, When shutting down an electrically controlled switch, the following steps are also included: When a signal to close the electronically controlled switch is received, the electronically controlled switch is closed after a set delay, allowing a fixed volume of fluid to be discharged from the upper cavity of the electronically controlled switch.

10. The automated liquid-liquid extraction and layer separation method according to claim 9, characterized in that, When the electronically controlled switch is turned off after a set delay, the set delay is statically set in advance based on the known density value of the discharged fluid.

11. The automated liquid-liquid extraction and layer separation method according to claim 9, characterized in that, When the electronically controlled switch is turned off after a set delay, the set delay is dynamically determined by looking up a table based on the real-time density detection value of the discharged fluid.

12. An automated liquid-liquid extraction and separation device, characterized in that, include: The light intensity signal acquisition module is used to acquire the light intensity signal obtained by the photoelectric detection unit acting on the fluid in the drain pipe in real time at a preset frequency according to a preset optical path. The fluctuation degree calculation module is used to calculate the real-time amplitude of the light intensity signal and the degree of real-time amplitude change within a preset window range; A fluid state recognition module is used to automatically identify the current fluid state at the relative photoelectric detection unit in the drain pipe according to the type of change, wherein the current fluid state includes pure liquid phase, emulsion layer and phase change interface; The switch control module is used to automatically control the opening and closing of the electronically controlled switch device located on the drain pipe and downstream of the photoelectric detection unit according to the identified current fluid state, so as to realize the liquid-liquid extraction and stratification separation.

13. An electronic device, the electronic device comprising: A memory, a processor, and a computer program stored in the memory and executable on the processor, characterized in that, when the processor executes the computer program, it implements the automated liquid-liquid extraction and separation method as described in any one of claims 1 to 11.

14. A computer-readable storage medium having a computer program stored thereon, characterized in that, When the computer program is executed by the processor, it implements the automated liquid-liquid extraction and separation method as described in any one of claims 1 to 11.

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