Solvent extraction equipment and method for physical and chemical inspection

Abstract

The invention provides solvent extraction equipment and method for physical and chemical inspection. Volume change data and temperature change data of a solution to be treated in the nitrogen blowing concentration process are collected in real time through an intelligent sensor; identifying bubble interference generated on the liquid surface of the to-be-treated solution in the nitrogen blowing concentration process according to fluctuation characteristics of the volume change data, and determining the loss amount of the to-be-treated solution in the nitrogen blowing concentration process through the bubble interference; determining deviation characteristics of latent heat change in the nitrogen blowing concentration process according to the environmental parameters and the temperature change data, and determining model gain of a concentration rate tracking model in the nitrogen blowing concentration process based on the deviation characteristics; adjusting the nitrogen flow of a nitrogen blowing needle head in the nitrogen blowing concentration process according to the model gain and the loss amount so as to complete the nitrogen blowing concentration of the solution and obtain a solution sample for physical and chemical inspection. By adopting the scheme provided by the invention, the nitrogen flow can be adjusted in real time in nitrogen blowing concentration, so that the loss of a solution sample in physical and chemical inspection is reduced.

Description

Technical Field

[0001] The present application relates to the technical field of sample preparation, and more specifically, to a solvent extraction device and method for physical and chemical testing. Background Art

[0002] Physical and chemical testing refers to the process of detecting and analyzing the physical and chemical properties of substances through scientific instruments or chemical methods. Solvent extraction is a commonly used method for separating and enriching target substances in physical and chemical testing. The solvent's solubility and selectivity are used to extract specific components from the sample for subsequent qualitative or quantitative analysis. Concentration is an important step in solvent extraction, and its purpose is to increase the concentration of the solution sample and reduce its volume.

[0003] In the prior art, methods commonly used for solution concentration include rotary evaporation, nitrogen blowing concentration, freeze drying and vacuum concentration. Among them, nitrogen blowing concentration is widely used in various physical and chemical testing occasions because of its good protection of the thermal sensitivity of solution samples and its suitability for trace solution samples. However, in actual applications of nitrogen blowing concentration, the viscosity and other properties of the solution will continue to change with the concentration process. When the solution viscosity is high and the nitrogen flow rate is high, the nitrogen gas cannot diffuse, and part of the nitrogen flow will enter the liquid surface of the solution to form bubbles, which will cause problems such as solution splashing or too slow concentration, and then cause the loss of samples for physical and chemical testing. Therefore, how to adjust the nitrogen flow rate in real time during nitrogen blowing concentration to reduce the loss of solution samples in physical and chemical testing has become a difficult problem faced by the industry. Summary of the invention

[0004] The present application provides a solvent extraction device and method for physical and chemical testing, which can adjust the nitrogen flow rate in real time during nitrogen blowing concentration to reduce the loss of solution samples in physical and chemical testing.

[0005] In a first aspect, the present application provides a method for nitrogen blowing concentration of a solution, wherein a solvent extraction device for physical and chemical testing performs nitrogen blowing concentration of a solution, wherein the solvent extraction device comprises: a concentration container, a nitrogen valve, an intelligent sensor and a nitrogen blowing needle, and the method comprises: The extracted solution is filtered and placed in the concentration container to obtain a solution to be treated; Opening the nitrogen valve to start nitrogen blowing and concentration, and collecting the volume change data and temperature change data of the solution to be treated in real time during the nitrogen blowing and concentration process through the intelligent sensor; Identifying bubble interference generated on the liquid surface of the solution to be treated during nitrogen blowing and concentration according to the fluctuation characteristics of the volume change data, and determining the loss amount of the solution to be treated during the nitrogen blowing and concentration process through the bubble interference; Acquire environmental parameters collected by the intelligent sensor during the nitrogen blowing concentration process, determine deviation characteristics of latent heat change during the nitrogen blowing concentration process according to the environmental parameters and the temperature change data, and determine a model gain of a concentration rate tracking model during the nitrogen blowing concentration process based on the deviation characteristics; The nitrogen flow rate of the nitrogen blowing needle during the nitrogen blowing concentration process is adjusted according to the model gain and the loss amount, thereby completing the nitrogen blowing concentration of the solution and obtaining a solution sample for physical and chemical testing.

[0006] In some embodiments, identifying the bubble interference generated on the liquid surface of the solution to be treated during the nitrogen blowing concentration process according to the fluctuation characteristics of the volume change data specifically includes: determining a fluctuation characteristic of the volume change data; Determining the volatilization rate sequence of the solution to be treated during the nitrogen blowing concentration process according to the volume change data; The bubble interference generated on the liquid surface of the solution to be treated during the nitrogen blowing concentration process is determined according to the volatilization rate sequence and the fluctuation characteristics.

[0007] In some embodiments, determining the loss amount of the solution to be treated during the nitrogen blowing concentration process by the bubble interference specifically includes: Determining the state vector of the solution to be treated at the current moment; Determine a plurality of state points in a state space according to the bubble interference and the state vector; The loss amount of the solution to be treated during the nitrogen blowing concentration process is determined according to all state points.

[0008] In some embodiments, determining the deviation characteristics of the latent heat change during the nitrogen blowing concentration process according to the environmental parameters and the temperature change data specifically includes: Determine the temperature difference at the current moment according to the temperature change data; Determining a latent heat coefficient of volatilization according to the environmental parameters; Determining a plurality of prediction candidate states according to the latent heat coefficient of evaporation and the temperature difference at a current moment; The deviation characteristics of the latent heat change during nitrogen blowing and enrichment are determined based on all prediction candidate states.

[0009] In some embodiments, adjusting the nitrogen flow rate of the nitrogen blowing needle during the nitrogen blowing concentration process according to the model gain and the loss amount specifically includes: Determining a predicted concentration rate of the solvent to be processed based on the model gain and the loss amount; The predicted concentration rate is compared with a preset target concentration rate, and if the predicted concentration rate is greater than the preset target concentration rate, the nitrogen flow rate of the nitrogen blowing needle is reduced during the nitrogen blowing concentration process; If the predicted concentration rate is less than the preset target concentration rate, increasing the nitrogen flow rate of the nitrogen blowing needle during the nitrogen blowing concentration process; If the predicted concentration rate is equal to the preset target concentration rate, the nitrogen flow rate of the nitrogen blowing needle during the nitrogen blowing concentration process is not adjusted.

[0010] In some embodiments, the smart sensor is an integrated sensor for measuring the temperature and volume of the solution in the concentration container and the temperature and atmospheric pressure of the external environment.

[0011] In some embodiments, determining the model gain of the enrichment rate tracking model in the nitrogen blowing enrichment process based on the deviation feature specifically includes: determining a plurality of tracking points according to the deviation characteristics; The model gain of the enrichment rate tracking model during nitrogen blowing enrichment is determined based on all tracking points.

[0012] In a second aspect, the present application provides a solvent extraction device for physical and chemical testing, the solvent extraction device for physical and chemical testing includes a nitrogen blowing concentration processing unit, and the nitrogen blowing concentration processing unit includes: A collection module, for filtering the extracted solution and placing it in the concentration container to obtain a solution to be treated, opening the nitrogen valve to start nitrogen blowing and concentration, and instructing the intelligent sensor to collect volume change data and temperature change data of the solution to be treated in real time during the nitrogen blowing and concentration process; A processing module, used for identifying the bubble interference generated on the liquid surface of the solution to be treated during the nitrogen blowing concentration process according to the fluctuation characteristics of the volume change data, and determining the loss amount of the solution to be treated during the nitrogen blowing concentration process through the bubble interference; The processing module is also used to obtain environmental parameters collected by the intelligent sensor during the nitrogen blowing concentration process, determine the deviation characteristics of the latent heat change during the nitrogen blowing concentration process according to the environmental parameters and the temperature change data, and determine the model gain of the concentration rate tracking model during the nitrogen blowing concentration process based on the deviation characteristics; The execution module is used to adjust the nitrogen flow rate of the nitrogen blowing needle during the nitrogen blowing concentration process according to the model gain and the loss amount, thereby completing the nitrogen blowing concentration of the solution and obtaining a solution sample for physical and chemical testing.

[0013] In a third aspect, the present application provides a computer device, comprising a memory and a processor, wherein the memory stores codes, and the processor is configured to obtain the codes and execute the above-mentioned nitrogen blowing concentration method for the solution.

[0014] In a fourth aspect, the present application provides a computer-readable storage medium, wherein the computer-readable storage medium stores a computer program, and when the computer program is executed by a processor, the nitrogen blowing concentration method of the solution is implemented.

[0015] The technical solution provided by the embodiments disclosed in this application has the following beneficial effects: In the solvent extraction equipment and method for physical and chemical testing provided by the present application, the extracted solution is first filtered and then placed in the concentration container to obtain a solution to be treated; the nitrogen valve is opened to start nitrogen blowing and concentration, and the volume change data and temperature change data of the solution to be treated during the nitrogen blowing and concentration process are collected in real time by the intelligent sensor; the bubble interference generated on the liquid surface of the solution to be treated during the nitrogen blowing and concentration process is identified according to the fluctuation characteristics of the volume change data, and the loss amount of the solution to be treated during the nitrogen blowing and concentration process is determined according to the bubble interference; the environmental parameters collected by the intelligent sensor during the nitrogen blowing and concentration process are obtained, the deviation characteristics of the latent heat change during the nitrogen blowing and concentration process are determined according to the environmental parameters and the temperature change data, and the model gain of the concentration rate tracking model during the nitrogen blowing and concentration process is determined based on the deviation characteristics; the nitrogen flow rate of the nitrogen blowing needle during the nitrogen blowing and concentration process is adjusted according to the model gain and the loss amount, thereby completing the nitrogen blowing and concentration of the solution to obtain a solution sample for physical and chemical testing.

[0016] It can be seen that the present application identifies the bubble interference generated on the liquid surface of the solution to be treated through the uncertainty of the volume change of the solution to be treated (i.e., the fluctuation characteristics), and then quantifies the loss amount in the nitrogen blowing concentration process through the bubble interference, that is, determines the viscosity characteristics of the solution to be treated, and then introduces the uncertainty of temperature change (i.e., the deviation characteristics of latent heat change) to determine the model gain of the concentration rate tracking model in the nitrogen blowing concentration process, that is, to correct the tracking model of the concentration rate of the solution to be treated when the temperature changes, and finally predicts the concentration rate of the solution to be treated by the loss amount and the model gain, and adjusts the nitrogen flow rate of the nitrogen blowing needle in the nitrogen blowing concentration process in real time based on the prediction result to ensure that the nitrogen flow rate in the nitrogen blowing concentration process is always adapted to the current temperature and solution viscosity, and avoids splashing of the solution to be treated during the nitrogen blowing concentration process. In summary, the scheme of the present application can adjust the nitrogen flow rate in real time during nitrogen blowing concentration to reduce the loss of solution samples in physical and chemical tests. BRIEF DESCRIPTION OF THE DRAWINGS

[0017] Figure 1 is an exemplary flow chart of a nitrogen blowing concentration method for a solution according to some embodiments of the present application; Figure 2 is a schematic structural diagram of a vacuum filtration device according to some embodiments of the present application; Figure 3is an exemplary flow chart of determining deviation characteristics according to some embodiments of the present application; Figure 4 is a schematic structural diagram of a nitrogen blowing concentration processing unit according to some embodiments of the present application; Figure 5 It is a structural schematic diagram of a computer device for implementing a nitrogen blowing concentration method for a solution according to some embodiments of the present application. DETAILED DESCRIPTION

[0018] In order to better understand the technical solution of the present application, the technical solution of the present application will be described in detail below in conjunction with the accompanying drawings and specific implementation methods.

[0019] refer to Figure 1 , which is an exemplary flow chart of a nitrogen blowing concentration method for a solution according to some embodiments of the present application, wherein the nitrogen blowing concentration method 100 for the solution mainly comprises the following steps: In step 101, the extracted solution is filtered and placed in the concentration container to obtain a solution to be treated.

[0020] In specific implementation, the extracted solution is filtered and placed in the concentrating container to obtain the solution to be treated, which can be achieved in the following manner, namely: the extracted solution can be filtered through a vacuum filtration device, and the filtered solution is drained into the concentrating container, and the solution placed in the concentrating container is used as the solution to be treated.

[0021] It should be noted that the vacuum filtration device in the present application is a glass sand core filtration device.

[0022] In some embodiments, reference Figure 2 , this figure is a schematic structural diagram of a vacuum filtration device according to some embodiments of the present application, the vacuum filtration device includes: a triangular flask 1, a connecting pipe 2, a filter head 3, a filter element 4, a vacuum pump 5, an exhaust interface 6, a No. 1 sand core 7, a left scale line 8, a right scale line 9, a filter cup 10 and a No. 1 sand core 11.

[0023] In step 102, the nitrogen valve is opened to start nitrogen blowing and concentration, and the volume change data and temperature change data of the solution to be treated during the nitrogen blowing and concentration process are collected in real time by the intelligent sensor.

[0024] In specific implementation, the real-time collection of the volume change data and temperature change data of the solution to be treated during the nitrogen blowing concentration process by the intelligent sensor can be achieved in the following manner, namely: at every preset sampling interval, the temperature value and volume value of the solution to be treated during the nitrogen blowing concentration process are collected by the intelligent sensor, and then all the collected temperature values ​​are sorted in the order of collection, and the obtained sequence is used as the temperature change data of the solution to be treated during the nitrogen blowing concentration process, and then all the collected volume values ​​are sorted in the order of collection, and the obtained sequence is used as the volume change data of the solution to be treated during the nitrogen blowing concentration process, wherein the sampling interval is a parameter preset according to actual needs. For example, in the present application, the sampling interval can be preset to 1 second.

[0025] It should be noted that the intelligent sensor in the present application is an integrated sensor for measuring the temperature and volume of the solution in the concentration container and the temperature and atmospheric pressure of the external environment.

[0026] In step 103, bubble interference generated on the liquid surface of the solution to be treated during the nitrogen blowing concentration process is identified according to the fluctuation characteristics of the volume change data, and the loss amount of the solution to be treated during the nitrogen blowing concentration process is determined through the bubble interference.

[0027] In some embodiments, identifying the bubble interference generated on the liquid surface of the solution to be treated during nitrogen blowing concentration according to the fluctuation characteristics of the volume change data can be achieved by the following steps: determining a fluctuation characteristic of the volume change data; Determining the volatilization rate sequence of the solution to be treated during the nitrogen blowing concentration process according to the volume change data; Determining the abnormal interference amount in the nitrogen blowing concentration process according to the volatilization rate sequence; The bubble interference generated on the liquid surface of the solution to be treated during the nitrogen blowing concentration process is determined according to the abnormal interference amount and the fluctuation characteristics.

[0028] It should be noted that the fluctuation characteristic in the present application is a parameter value that measures the fluctuation degree of the volume change of the solution to be treated during the nitrogen blowing and concentration process. The larger the fluctuation characteristic, the greater the fluctuation degree of the volume change of the solution to be treated during the nitrogen blowing and concentration process. The smaller the fluctuation characteristic, the smaller the fluctuation degree of the volume change of the solution to be treated during the nitrogen blowing and concentration process. As a preferred embodiment, the fluctuation characteristic of the volume change data determined in the present application can be achieved in the following manner, namely: taking the variance of the sequence corresponding to the volume change data as the fluctuation characteristic of the volume change data.

[0029] In specific implementation, determining the volatilization rate sequence of the solution to be treated in the nitrogen blowing and concentration process according to the volume change data can be achieved in the following manner, namely: first, selecting a volume value in the sequence corresponding to the volume change data as the selected volume value, subtracting the next volume value of the selected volume value in the sequence corresponding to the volume change data from the selected volume value, then dividing the value obtained by the subtraction by the sampling interval when the volume change data is collected, and taking the value obtained by dividing by the sampling interval as the volatilization rate corresponding to the selected volume value, and continuing to determine the volatilization rates of the remaining volume values ​​in the sequence corresponding to the volume change data, and then, sorting all the volatilization rates according to the order of the corresponding volume values ​​in the sequence corresponding to the volume change data, and finally, taking the obtained sequence as the volatilization rate sequence of the solution to be treated in the nitrogen blowing and concentration process.

[0030] It should be noted that the volatilization rate sequence in the present application is a sequence representing the change of the volatilization rate of the solvent in the solution over time during the nitrogen blowing concentration process.

[0031] In addition, it should be noted that the abnormal interference amount in the present application is a parameter value that measures the degree of interference to the concentration rate during the nitrogen blowing concentration process. The larger the abnormal interference amount, the more interference to the concentration rate during the nitrogen blowing concentration process. The smaller the abnormal interference amount, the less interference to the concentration rate during the nitrogen blowing concentration process. As a preferred embodiment, the abnormal interference amount in the nitrogen blowing concentration process can be determined according to the volatilization rate sequence in the present application. The following method can be used to achieve this, namely: the variance of the volatilization rate sequence is used as the abnormal interference amount in the nitrogen blowing concentration process.

[0032] In specific implementation, the bubble interference generated on the liquid surface of the solution to be treated during the nitrogen blowing concentration process is determined according to the volatilization rate sequence and the fluctuation characteristics, which can be achieved in the following manner: first, the fluctuation characteristics are taken as A, and the abnormal interference amount is taken as B, and then the covariance C of the corresponding sequence of volume change data and the volatilization rate sequence is calculated, and finally, the matrix [A, C; C, B] is used as the quantization matrix of the bubble interference generated on the liquid surface of the solution to be treated during the nitrogen blowing concentration process.

[0033] It should be noted that the fluctuation characteristic in the present application is a quantitative matrix that describes the uncertainty of the volatilization rate of the solution to be treated during the nitrogen blowing concentration process. The fluctuation is caused by the mismatch of the nitrogen flow rate due to the change in the solvent content in the solution. When this fluctuation occurs, bubbles will appear on the surface of the solution, resulting in solution splashing and sample loss.

[0034] In some embodiments, determining the loss of the solution to be treated during the nitrogen blowing concentration process by the bubble interference can be achieved by the following steps: Determining the state vector of the solution to be treated at the current moment; Determine a plurality of state points in a state space according to the bubble interference and the state vector; The loss amount of the solution to be treated during the nitrogen blowing concentration process is determined according to all state points.

[0035] In specific implementation, the state vector of the solution to be treated at the current moment can be determined in the following manner: first, the average value a of all volume values ​​in the sequence corresponding to the volume change data is calculated, then the average value b of all volatilization rates in the volatilization rate sequence is calculated, and finally, the vector [a; b] is used as the state vector of the solution to be treated at the current moment.

[0036] It should be noted that the state vector in this application is a vector that describes the state of the solution to be treated at the current moment.

[0037] In a specific implementation, determining multiple state points in the state space according to the bubble interference and the state vector can be achieved in the following manner, namely: first, decomposing the quantization matrix of the bubble interference into an upper triangular matrix and a lower triangular matrix by the Cholesky decomposition in the prior art, and then obtaining all unit basis vectors in the two-dimensional space. For each unit basis vector, multiplying the decomposed upper triangular matrix by the unit basis vector, and adding the obtained vector to the state vector. Finally, the added vector is used as the state point of the unit basis vector in the state space, thereby obtaining the state point of each unit basis vector in the state space.

[0038] It should be noted that the state point in the present application is the point represented in the state space by the vector describing the state of the volume of the solution to be treated at the next moment. Since the change in the volume of the solution to be treated at the current moment fluctuates, that is, is uncertain, there are multiple situations for the state of the volume of the solution to be treated at the next moment, that is, there are multiple state points.

[0039] In specific implementation, determining the loss amount of the solution to be treated during the nitrogen blowing concentration process according to all state points can be achieved in the following manner, namely: first, calculating the covariance matrix of all state points, and then using the determinant of the covariance matrix as the loss amount of the solution to be treated during the nitrogen blowing concentration process.

[0040] It should be noted that the loss amount in this application is a parameter value for measuring the degree of sample loss in the solution to be treated during the nitrogen blowing and concentration process. The larger the loss amount, the more sample loss in the solution to be treated during the nitrogen blowing and concentration process. The smaller the loss amount, the less sample loss in the solution to be treated during the nitrogen blowing and concentration process. The loss is caused by splashing of the solution due to incorrect nitrogen flow.

[0041] In step 104, environmental parameters collected by the intelligent sensor during the nitrogen blowing concentration process are obtained, deviation characteristics of latent heat change during the nitrogen blowing concentration process are determined according to the environmental parameters and the temperature change data, and a model gain of a concentration rate tracking model during the nitrogen blowing concentration process is determined based on the deviation characteristics.

[0042] In specific implementation, the environmental parameters collected by the intelligent sensor during the nitrogen blowing and concentration process can be obtained in the following manner, namely: at every preset sampling interval, the temperature value and atmospheric pressure value of the external environment during the nitrogen blowing and concentration process are collected by the intelligent sensor, and then the average value of all the collected temperature values ​​is used as the average temperature, and the average value of all the collected atmospheric pressure values ​​is used as the average atmospheric pressure. Finally, the average temperature and the average atmospheric pressure are used as the external environmental parameters during the nitrogen blowing and concentration process.

[0043] It should be noted that the environmental parameters in this application refer to the average temperature and average atmospheric pressure of the external environment during the nitrogen blowing concentration process.

[0044] In some embodiments, reference Figure 3 , which is an exemplary flow chart of determining deviation characteristics according to some embodiments of the present application. In the present application, the deviation characteristics of the latent heat change during nitrogen blowing concentration can be determined according to the environmental parameters and the temperature change data by using the following steps: In step 1041, the temperature difference at the current moment is determined according to the temperature change data; In step 1042, a latent heat coefficient of volatilization is determined according to the environmental parameters; In step 1043, a plurality of prediction candidate states are determined according to the latent heat coefficient of evaporation and the temperature difference at the current moment; In step 1044, deviation characteristics of latent heat changes during nitrogen purge concentration are determined based on all prediction candidate states.

[0045] It should be noted that the temperature difference in the present application refers to the temperature difference between the current moment and the previous moment of the solution to be treated. As a preferred embodiment, the temperature difference at the current moment can be determined according to the temperature change data in the present application in the following manner, namely: subtract the last two temperature values ​​in the sequence corresponding to the temperature change data, and use the obtained difference as the temperature difference at the current moment.

[0046] In specific implementation, determining the latent heat coefficient of volatilization according to the environmental parameters can be achieved in the following manner, namely: first, obtaining the average temperature and average atmospheric pressure in the environmental parameters, obtaining the latent heat of vaporization of the solvent in the solution to be treated at the average temperature and average atmospheric pressure by querying the latent heat of vaporization table, then obtaining the initial mass of the solution to be treated, then multiplying the density of the solvent in the solution to be treated by the latent heat of vaporization and dividing the obtained value by the product of the initial mass and the specific heat capacity of the solvent in the solution to be treated, and finally, using the obtained quotient as the latent heat coefficient of volatilization.

[0047] It should be noted that the latent heat of volatilization coefficient in the present application is a parameter value that represents the influence of the latent heat of volatilization of the solvent in the solution to be treated on the temperature change. The larger the latent heat of volatilization coefficient, the greater the influence of the latent heat of volatilization of the solvent in the solution to be treated on the temperature change, that is, the greater the temperature change of the solution to be treated per unit volume of solvent volatilized. The smaller the latent heat of volatilization coefficient, the smaller the influence of the latent heat of volatilization of the solvent in the solution to be treated on the temperature change, that is, the smaller the temperature change of the solution to be treated per unit volume of solvent volatilized.

[0048] In specific implementation, multiple prediction candidate states can be determined according to the latent heat coefficient of volatilization and the temperature difference at the current moment. The following method is adopted, namely: first, for each state point, the time transfer matrix is ​​multiplied by square root of 2 and then multiplied with the state point to obtain vector Q. Then, the temperature transfer matrix is ​​multiplied by the temperature difference at the current moment to obtain vector P. Subsequently, vector P is divided by the latent heat coefficient of volatilization and then added to vector Q. Finally, the added vector is used as the prediction candidate state, thereby obtaining the prediction candidate state of each state point, wherein the time transfer matrix is ​​[1, t; 0, 1], the temperature transfer matrix is ​​[lnt; 1 / t], and t is the sampling interval for collecting the temperature change data and volume change data of the solution to be treated during the nitrogen blowing concentration process.

[0049] It should be noted that the predicted candidate state in the present application is the predicted state of the volume of the solution to be processed at the next moment, and the predicted candidate state is the predicted state obtained after introducing the uncertainty of temperature change.

[0050] In specific implementation, the deviation characteristics of the latent heat change during the nitrogen blowing concentration process are determined based on all the prediction candidate states. The following method can be used, namely: first, the average vector of all the prediction candidate states is used as the predicted concentration state of the solution to be treated. Then, for each prediction candidate state, the predicted concentration state is subtracted from the predicted candidate state to obtain a deviation vector. Then, the deviation vector is multiplied by the transpose of the deviation vector, and the obtained matrix is ​​used as a prediction deviation matrix to obtain multiple prediction deviation matrices. Then, all the prediction deviation matrices are added and divided by the total number of prediction deviation matrices. Finally, the matrix obtained after the division is used as the deviation characteristic of the latent heat change during the nitrogen blowing concentration process.

[0051] It should be noted that the deviation characteristic in the present application is a quantitative matrix describing the change in latent heat in the solution to be treated caused by the volatilization of the solvent during the nitrogen blowing concentration process.

[0052] In some embodiments, determining the model gain of the enrichment rate tracking model in the nitrogen purge enrichment process based on the deviation feature can be implemented by the following steps: determining a plurality of tracking points according to the deviation characteristics; The model gain of the enrichment rate tracking model during nitrogen blowing enrichment is determined based on all tracking points.

[0053] In specific implementation, determining multiple tracking points based on the deviation features can be achieved in the following manner, namely: first, decomposing the matrix of the deviation features into an upper triangular matrix and a lower triangular matrix through the Cholesky decomposition in the prior art, then obtaining all unit basis vectors in the two-dimensional space, and for each unit basis vector, multiplying the decomposed upper triangular matrix with the unit basis vector, and adding the obtained vector to the vector of the predicted concentrated state, and finally, using the added vector as the tracking point, thereby obtaining multiple tracking points.

[0054] It should be noted that the tracking point in the present application is the point represented by the vector in the state space when tracking the change of the concentration rate after introducing the uncertainty of temperature.

[0055] In specific implementation, the model gain of the enrichment rate tracking model in the nitrogen blowing enrichment process can be determined according to all tracking points. The following method is used, namely: first, the covariance matrix of all tracking points is calculated, then all state points are obtained, and the cross-covariance matrix between all tracking points and all state points is calculated. Subsequently, the covariance matrix is ​​multiplied by the inverse matrix of the cross-covariance matrix, and the obtained value is used as the model gain.

[0056] It should be noted that the model gain in the present application is a parameter used to adjust the predicted value of the concentration rate after introducing the uncertainty of temperature.

[0057] In addition, it should be noted that the concentration rate tracking model in the present application refers to a model that predicts the concentration rate through volume change data and temperature change data. As a preferred embodiment, the tracking model is expressed as: predicted concentration rate = [0,1] * (model gain * prediction error * loss amount + predicted concentration state), wherein the predicted concentration state is the average vector of all predicted candidate states, and the prediction error refers to the difference between the average vector of all tracking points and the state vector of the solution to be treated at the current moment. The concentration rate tracking model corrects the predicted concentration state by introducing loss amount and model gain, and can adjust the prediction result in real time according to the concentration process of the solution to be treated to obtain a more accurate predicted concentration rate.

[0058] In step 105, the nitrogen flow rate of the nitrogen blowing needle during the nitrogen blowing concentration process is adjusted according to the model gain and the loss amount, thereby completing the nitrogen blowing concentration of the solution and obtaining a solution sample for physical and chemical testing.

[0059] In some embodiments, adjusting the nitrogen flow rate of the nitrogen blowing needle during the nitrogen blowing concentration process according to the model gain and the loss amount can be achieved by the following steps: Determining a predicted concentration rate of the solvent to be processed based on the model gain and the loss amount; The predicted concentration rate is compared with a preset target concentration rate, and if the predicted concentration rate is greater than the preset target concentration rate, the nitrogen flow rate of the nitrogen blowing needle is reduced during the nitrogen blowing concentration process; If the predicted concentration rate is less than the preset target concentration rate, increasing the nitrogen flow rate of the nitrogen blowing needle during the nitrogen blowing concentration process; If the predicted concentration rate is equal to the preset target concentration rate, the nitrogen flow rate of the nitrogen blowing needle during the nitrogen blowing concentration process is not adjusted.

[0060] In specific implementation, the predicted concentration rate of the solvent to be treated can be determined based on the model gain and the loss amount in the following manner, namely: first, the average vector of all tracking points is calculated, and then the state vector of the solution to be treated at the current moment is subtracted from the average vector, and the obtained value is multiplied by the loss amount, and then the obtained quotient is multiplied by the model gain, and the multiplied value is added to the average vector of all predicted candidate states, and finally the second element in the vector obtained after the addition is used as the predicted concentration rate of the solvent to be treated.

[0061] It should be noted that the predicted concentration rate in the present application refers to the predicted concentration rate of the solution to be treated at the next moment.

[0062] It should be noted that the target concentration rate in the present application is preset according to the properties of different solvents and actual needs. The solutions used for physical and chemical testing are usually small volume samples, so the target concentration rate is often preset to a value between 1ml / min-10ml / min. For example, in the present application, the target concentration rate can be set to 5ml / min.

[0063] In specific implementation, if the predicted concentration rate is greater than the preset target concentration rate, reducing the nitrogen flow rate of the nitrogen blowing needle during the nitrogen blowing concentration process can be achieved in the following manner, namely: the nitrogen flow rate of the nitrogen blowing needle can be reduced by 10 ml / min when the predicted concentration rate is greater than the preset target concentration rate.

[0064] In specific implementation, if the predicted concentration rate is less than the preset target concentration rate, increasing the nitrogen flow rate of the nitrogen blowing needle during the nitrogen blowing concentration process can be achieved in the following manner, namely: when the predicted concentration rate is less than the preset target concentration rate, the nitrogen flow rate of the nitrogen blowing needle can be increased by 10 ml / min.

[0065] In addition, in another aspect of the present application, in some embodiments, the present application provides a solvent extraction device for physical and chemical testing, the solvent extraction device for physical and chemical testing includes a nitrogen blowing concentration processing unit, referring to Figure 4 , which is a schematic diagram of the structure of a nitrogen blowing concentration processing unit according to some embodiments of the present application, the nitrogen blowing concentration processing unit 400 includes: a collection module 401, a processing module 402 and an execution module 403, which are described as follows: The acquisition module 401 in the present application is mainly used to filter the extracted solution and place it in the concentration container to obtain a solution to be treated, open the nitrogen valve to start nitrogen blowing and concentration, and instruct the intelligent sensor to collect the volume change data and temperature change data of the solution to be treated in real time during the nitrogen blowing and concentration process; Processing module 402, in the present application, the processing module 402 is mainly used to identify the bubble interference generated on the liquid surface of the solution to be treated during the nitrogen blowing concentration process according to the fluctuation characteristics of the volume change data, and determine the loss amount of the solution to be treated during the nitrogen blowing concentration process through the bubble interference; It should be noted that the processing module 402 in the present application is also used to obtain the environmental parameters collected by the intelligent sensor during the nitrogen blowing concentration process, determine the deviation characteristics of the latent heat change during the nitrogen blowing concentration process according to the environmental parameters and the temperature change data, and determine the model gain of the concentration rate tracking model during the nitrogen blowing concentration process based on the deviation characteristics; Execution module 403, in the present application, execution module 403 is mainly used to adjust the nitrogen flow rate of the nitrogen blowing needle during the nitrogen blowing concentration process according to the model gain and the loss amount, thereby completing the nitrogen blowing concentration of the solution and obtaining a solution sample for physical and chemical testing.

[0066] In addition, the present application also provides a computer device, which includes a memory and a processor, wherein the memory stores codes, and the processor is configured to obtain the codes and execute the above-mentioned nitrogen blowing concentration method for the solution.

[0067] In some embodiments, reference Figure 5 , which is a schematic diagram of the structure of a computer device for implementing a nitrogen blowing concentration method for a solution according to some embodiments of the present application. The nitrogen blowing concentration method for a solution in the above embodiment can be performed by Figure 5The computer device 500 shown in the figure is implemented, and the computer device 500 includes at least one processor 501, a communication bus 502, a memory 503 and at least one communication interface 504.

[0068] The processor 501 may be a general-purpose central processing unit (CPU) or an application-specific integrated circuit (ASIC).

[0069] The communication bus 502 may be used to transmit information between the above-mentioned components.

[0070] The memory 503 may be a read-only memory (ROM) or other types of static storage devices that can store static information and instructions, a random access memory (RAM) or other types of dynamic storage devices that can store information and instructions, or an electrically erasable programmable read-only memory (EEPROM), a compact disc read-only memory (CD-ROM) or other optical disc storage, an optical disc storage (including a compressed optical disc, a laser disc, an optical disc, a digital versatile disc, a Blu-ray disc, etc.), a magnetic disk or other magnetic storage device, or any other medium that can be used to carry or store the desired program code in the form of an instruction or data structure and can be accessed by a computer, but is not limited thereto. The memory 503 may exist independently and be connected to the processor 501 via the communication bus 502. The memory 503 may also be integrated with the processor 501.

[0071] The memory 503 is used to store the program code for executing the solution of the present application, and the execution is controlled by the processor 501. The processor 501 is used to execute the program code stored in the memory 503. The program code may include one or more software modules. The nitrogen blowing concentration method of the solution in the above embodiment can be implemented by the processor 501 and one or more software modules in the program code in the memory 503.

[0072] The communication interface 504 uses any transceiver or other device for communicating with other devices or communication networks, such as Ethernet, radio access network (RAN), wireless local area networks (WLAN), etc.

[0073] In a specific implementation, as an embodiment, a computer device may include multiple processors, each of which may be a single-CPU processor or a multi-CPU processor. The processor here may refer to one or more devices, circuits, and / or processing cores for processing data (e.g., computer program instructions).

[0074] The above-mentioned computer device may be a general-purpose computer device or a special-purpose computer device. In a specific implementation, the computer device may be a desktop computer, a portable computer, a network server, a personal digital assistant (PDA), a mobile phone, a tablet computer, a wireless terminal device, a communication device or an embedded device. The embodiment of the present application does not limit the type of computer device.

[0075] In addition, the present application also provides a computer-readable storage medium, wherein the computer-readable storage medium stores a computer program, and when the computer program is executed by a processor, the above-mentioned nitrogen blowing concentration method of the solution is implemented.

[0076] In summary, in the solvent extraction equipment and method for physical and chemical testing disclosed in the embodiments of the present application, first, the extracted solution is filtered and placed in the concentration container to obtain a solution to be treated; the nitrogen valve is opened to start nitrogen blowing and concentration, and the volume change data and temperature change data of the solution to be treated during the nitrogen blowing and concentration process are collected in real time by the intelligent sensor; the bubble interference generated on the liquid surface of the solution to be treated during the nitrogen blowing and concentration process is identified according to the fluctuation characteristics of the volume change data, and the loss amount of the solution to be treated during the nitrogen blowing and concentration process is determined by the bubble interference; the environmental parameters collected by the intelligent sensor during the nitrogen blowing and concentration process are obtained, and the deviation characteristics of the latent heat change during the nitrogen blowing and concentration process are determined according to the environmental parameters and the temperature change data, and the model gain of the concentration rate tracking model during the nitrogen blowing and concentration process is determined based on the deviation characteristics; the nitrogen flow rate of the nitrogen blowing needle during the nitrogen blowing and concentration process is adjusted according to the model gain and the loss amount, thereby completing the nitrogen blowing and concentration of the solution to obtain a solution sample for physical and chemical testing.

[0077] It can be seen that the present application identifies the bubble interference generated on the liquid surface of the solution to be treated through the uncertainty of the volume change of the solution to be treated (i.e., the fluctuation characteristics), and then quantifies the loss amount in the nitrogen blowing concentration process through the bubble interference, that is, determines the viscosity characteristics of the solution to be treated, and then introduces the uncertainty of temperature change (i.e., the deviation characteristics of latent heat change) to determine the model gain of the concentration rate tracking model in the nitrogen blowing concentration process, that is, to correct the tracking model of the concentration rate of the solution to be treated when the temperature changes, and finally predicts the concentration rate of the solution to be treated by the loss amount and the model gain, and adjusts the nitrogen flow rate of the nitrogen blowing needle in the nitrogen blowing concentration process in real time based on the prediction result to ensure that the nitrogen flow rate in the nitrogen blowing concentration process is always adapted to the current temperature and solution viscosity, and avoids splashing of the solution to be treated during the nitrogen blowing concentration process. In summary, the scheme of the present application can adjust the nitrogen flow rate in real time during nitrogen blowing concentration to reduce the loss of solution samples in physical and chemical tests.

[0078] Although the preferred embodiments of the present application have been described, those skilled in the art may make other changes and modifications to these embodiments once they have learned the basic creative concept. Therefore, the appended claims are intended to be interpreted as including the preferred embodiments and all changes and modifications falling within the scope of the present application.

[0079] Obviously, those skilled in the art can make various changes and modifications to the present application without departing from the spirit and scope of the present application. Thus, if these modifications and variations of the present application fall within the scope of the claims of the present application and their equivalents, the present application is also intended to include these modifications and variations.

Claims

1. A method for nitrogen blowing concentration of a solution, wherein the solvent extraction equipment for physical and chemical testing is used to carry out nitrogen blowing concentration of the solution, wherein: The solvent extraction equipment comprises: a concentration container, a nitrogen valve, an intelligent sensor and a nitrogen blowing needle, and is characterized in that it comprises: The extracted solution is filtered and placed in the concentration container to obtain a solution to be treated; Opening the nitrogen valve to start nitrogen blowing and concentration, and collecting the volume change data and temperature change data of the solution to be treated in real time during the nitrogen blowing and concentration process through the intelligent sensor; Identifying bubble interference generated on the liquid surface of the solution to be treated during nitrogen blowing and concentration according to the fluctuation characteristics of the volume change data, and determining the loss amount of the solution to be treated during the nitrogen blowing and concentration process through the bubble interference; Acquire environmental parameters collected by the intelligent sensor during the nitrogen blowing concentration process, determine deviation characteristics of latent heat change during the nitrogen blowing concentration process according to the environmental parameters and the temperature change data, and determine a model gain of a concentration rate tracking model during the nitrogen blowing concentration process based on the deviation characteristics; The nitrogen flow rate of the nitrogen blowing needle during the nitrogen blowing concentration process is adjusted according to the model gain and the loss amount, thereby completing the nitrogen blowing concentration of the solution and obtaining a solution sample for physical and chemical testing.

2. The method according to claim 1, characterized in that Identifying the bubble interference generated on the surface of the liquid of the solution to be treated during the nitrogen blowing concentration process according to the fluctuation characteristics of the volume change data specifically includes: determining a fluctuation characteristic of the volume change data; Determining the volatilization rate sequence of the solution to be treated during the nitrogen blowing concentration process according to the volume change data; The bubble interference generated on the liquid surface of the solution to be treated during the nitrogen blowing concentration process is determined according to the volatilization rate sequence and the fluctuation characteristics.

3. The method according to claim 1, characterized in that Determining the loss amount of the solution to be treated during the nitrogen blowing concentration process by the bubble interference specifically includes: Determining the state vector of the solution to be treated at the current moment; Determine a plurality of state points in a state space according to the bubble interference and the state vector; The loss amount of the solution to be treated during the nitrogen blowing concentration process is determined according to all state points.

4. The method according to claim 1, characterized in that Determining the deviation characteristics of the latent heat change during the nitrogen blowing concentration process according to the environmental parameters and the temperature change data specifically includes: Determine the temperature difference at the current moment according to the temperature change data; Determining a latent heat coefficient of volatilization according to the environmental parameters; Determining a plurality of prediction candidate states according to the latent heat coefficient of evaporation and the temperature difference at a current moment; The deviation characteristics of the latent heat change during nitrogen blowing and enrichment are determined based on all prediction candidate states.

5. The method according to claim 1, characterized in that Adjusting the nitrogen flow rate of the nitrogen blowing needle in the nitrogen blowing concentration process according to the model gain and the loss amount specifically includes: Determining a predicted concentration rate of the solvent to be processed based on the model gain and the loss amount; The predicted concentration rate is compared with a preset target concentration rate, and if the predicted concentration rate is greater than the preset target concentration rate, the nitrogen flow rate of the nitrogen blowing needle is reduced during the nitrogen blowing concentration process; If the predicted concentration rate is less than the preset target concentration rate, increasing the nitrogen flow rate of the nitrogen blowing needle during the nitrogen blowing concentration process; If the predicted concentration rate is equal to the preset target concentration rate, the nitrogen flow rate of the nitrogen blowing needle during the nitrogen blowing concentration process is not adjusted.

6. The method according to claim 1, characterized in that The intelligent sensor is an integrated sensor for measuring the temperature and volume of the solution in the concentration container and the temperature and atmospheric pressure of the external environment.

7. The method according to claim 1, characterized in that Determining the model gain of the enrichment rate tracking model in the nitrogen blowing enrichment process based on the deviation characteristics specifically includes: determining a plurality of tracking points according to the deviation characteristics; The model gain of the enrichment rate tracking model during nitrogen blowing enrichment is determined based on all tracking points.

8. A solvent extraction device for physical and chemical testing, the solvent extraction device for physical and chemical testing comprising a nitrogen blowing concentration processing unit, characterized in that: The nitrogen blowing concentration treatment unit comprises: A collection module, for filtering the extracted solution and placing it in the concentration container to obtain a solution to be treated, opening the nitrogen valve to start nitrogen blowing and concentration, and instructing the intelligent sensor to collect volume change data and temperature change data of the solution to be treated in real time during the nitrogen blowing and concentration process; A processing module, used for identifying the bubble interference generated on the liquid surface of the solution to be treated during the nitrogen blowing concentration process according to the fluctuation characteristics of the volume change data, and determining the loss amount of the solution to be treated during the nitrogen blowing concentration process through the bubble interference; The processing module is also used to obtain environmental parameters collected by the intelligent sensor during the nitrogen blowing concentration process, determine the deviation characteristics of the latent heat change during the nitrogen blowing concentration process according to the environmental parameters and the temperature change data, and determine the model gain of the concentration rate tracking model during the nitrogen blowing concentration process based on the deviation characteristics; The execution module is used to adjust the nitrogen flow rate of the nitrogen blowing needle during the nitrogen blowing concentration process according to the model gain and the loss amount, thereby completing the nitrogen blowing concentration of the solution and obtaining a solution sample for physical and chemical testing.

9. A computer device, characterized in that: The computer device comprises a memory and a processor, wherein the memory stores codes, and the processor is configured to obtain the codes and execute the nitrogen blowing concentration method for a solution according to any one of claims 1 to 7.

10. A computer-readable storage medium storing a computer program, characterized in that: When the computer program is executed by a processor, the method for nitrogen blowing and concentrating a solution according to any one of claims 1 to 7 is implemented.

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