Solvent extraction equipment and method for physical and chemical testing

Abstract

The present application provides a solvent extraction device and method for physical and chemical testing. The device collects volume change data and temperature change data of a solution to be treated during nitrogen blowing and concentration in real time through an intelligent sensor. The device identifies bubble interference generated on the liquid surface of the solution to be treated during the nitrogen blowing and concentration process based on the fluctuation characteristics of the volume change data, and determines the loss of the solution to be treated during the nitrogen blowing and concentration process based on the bubble interference. The device determines the deviation characteristics of the latent heat change during the nitrogen blowing and concentration process based on environmental parameters and temperature change data, and determines the model gain of a concentration rate tracking model during the nitrogen blowing and concentration process based on the deviation characteristics. The device adjusts the nitrogen flow rate of the nitrogen blowing needle during the nitrogen blowing and concentration process based on the model gain and loss amount, thereby completing the nitrogen blowing and concentration of the solution and obtaining a solution sample for physical and chemical testing. The solution of the present application can be used to adjust the nitrogen flow rate in real time during nitrogen blowing and concentration to reduce the loss of solution samples during physical and chemical testing.

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, the purpose of which is to increase the concentration of the solution sample and reduce its volume.

[0003] In the prior art, commonly used methods for solution concentration include rotary evaporation, nitrogen blow concentration, freeze drying, and vacuum concentration. Among them, nitrogen blow concentration is widely used in various physical and chemical testing occasions because it protects the heat sensitivity of solution samples well and is suitable for trace solution samples. However, in actual applications of nitrogen blow 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 slow concentration, and thus cause the loss of samples for physical and chemical testing. Therefore, how to adjust the nitrogen flow in real time during nitrogen blow 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 is used to nitrogen blow 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:

[0006] The extracted solution is filtered and placed in the concentration container to obtain a solution to be treated;

[0007] Opening the nitrogen valve to start nitrogen blowing and concentration, and collecting volume change data and temperature change data of the solution to be treated during the nitrogen blowing and concentration process in real time through the intelligent sensor;

[0008] Identifying 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 based on the bubble interference;

[0009] obtaining environmental parameters collected by the intelligent sensor during the nitrogen purge concentration process, determining deviation characteristics of latent heat change during the nitrogen purge concentration process based on the environmental parameters and the temperature change data, and determining a model gain of a concentration rate tracking model during the nitrogen purge concentration process based on the deviation characteristics;

[0010] 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.

[0011] In some embodiments, 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 specifically includes:

[0012] determining a fluctuation characteristic of the volume change data;

[0013] determining a volatilization rate sequence of the solution to be treated during nitrogen blowing and concentration according to the volume change data;

[0014] 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.

[0015] In some embodiments, determining the loss of the solution to be treated during the nitrogen purge concentration process by using the bubble interference specifically includes:

[0016] Determining the state vector of the solution to be processed at a current moment;

[0017] determining a plurality of state points in a state space according to the bubble interference and the state vector;

[0018] The loss amount of the solution to be treated during the nitrogen blowing and concentration process is determined according to all state points.

[0019] In some embodiments, determining the deviation characteristics of the latent heat change during the nitrogen purge concentration process based on the environmental parameters and the temperature change data specifically includes:

[0020] Determining the temperature difference at the current moment according to the temperature change data;

[0021] determining a latent heat coefficient of volatilization according to the environmental parameters;

[0022] Determining a plurality of candidate prediction states according to the latent heat coefficient of volatile matter and the temperature difference at a current moment;

[0023] The deviation characteristics of latent heat change during nitrogen purge concentration are determined based on all prediction candidate states.

[0024] 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 specifically includes:

[0025] determining a predicted concentration rate of the solvent to be processed based on the model gain and the loss amount;

[0026] comparing the predicted concentration rate with a preset target concentration rate, and 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;

[0027] 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;

[0028] 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.

[0029] In some embodiments, the smart sensor is an integrated sensor that measures the temperature and volume of the solution in the concentration container and the temperature and atmospheric pressure of the external environment.

[0030] In some embodiments, determining the model gain of the concentration rate tracking model during nitrogen purge concentration based on the deviation feature specifically includes:

[0031] determining a plurality of tracking points according to the deviation characteristics;

[0032] The model gain of the enrichment rate tracking model during nitrogen purge enrichment is determined based on all tracking points.

[0033] 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 and concentration processing unit, and the nitrogen blowing and concentration processing unit includes:

[0034] a collection module, configured 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 real-time volume change data and temperature change data of the solution to be treated during the nitrogen blowing and concentration process;

[0035] a processing module, configured to identify bubble interference generated on the liquid surface of the solution to be treated during the nitrogen blowing and concentration process based on the fluctuation characteristics of the volume change data, and determine the loss amount of the solution to be treated during the nitrogen blowing and concentration process based on the bubble interference;

[0036] The processing module is further configured to obtain environmental parameters collected by the intelligent sensor during the nitrogen purge concentration process, determine deviation characteristics of latent heat change during the nitrogen purge concentration process based on the environmental parameters and the temperature change data, and determine a model gain of a concentration rate tracking model during the nitrogen purge concentration process based on the deviation characteristics;

[0037] 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.

[0038] In a third aspect, the present application provides a computer device comprising a memory and a processor, wherein the memory stores a code, and the processor is configured to obtain the code and execute the above-mentioned nitrogen blow concentration method for the solution.

[0039] In a fourth aspect, the present application provides a computer-readable storage medium storing a computer program, which implements the above-mentioned nitrogen-blowing concentration method for a solution when executed by a processor.

[0040] The technical solutions provided by the embodiments disclosed in this application have the following beneficial effects:

[0041] In the solvent extraction equipment and method for physical and chemical testing provided in 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, 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.

[0042] 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. Subsequently, the uncertainty of temperature change (i.e., the deviation characteristics of latent heat change) is introduced to determine the model gain of the concentration rate tracking model in the nitrogen blowing concentration process, that is, the tracking model of the concentration rate of the solution to be treated is corrected when the temperature changes. Finally, the concentration rate of the solution to be treated is predicted by the loss amount and the model gain, and the nitrogen flow rate of the nitrogen blowing needle in the nitrogen blowing concentration process is adjusted 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, thereby avoiding splashing of the solution to be treated during the nitrogen blowing concentration process. In summary, the solution 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 testing. BRIEF DESCRIPTION OF THE DRAWINGS

[0043] Figure 1 is an exemplary flow chart of a method for nitrogen blowing concentration of a solution according to some embodiments of the present application;

[0044] Figure 2 is a schematic structural diagram of a vacuum filtration device according to some embodiments of the present application;

[0045] Figure 3 is an exemplary flow chart of determining deviation characteristics according to some embodiments of the present application;

[0046] Figure 4 is a schematic structural diagram of a nitrogen blowing and concentration processing unit according to some embodiments of the present application;

[0047] Figure 5 It is a structural schematic diagram of a computer device for implementing a nitrogen blow concentration method for a solution according to some embodiments of the present application. DETAILED DESCRIPTION

[0048] 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 with reference to the accompanying drawings and specific implementation methods.

[0049] 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. The nitrogen blowing concentration method 100 for a solution mainly includes the following steps:

[0050] In step 101, the extracted solution is filtered and then placed in the concentration container to obtain a solution to be treated.

[0051] In a specific implementation, the extracted solution is filtered and placed in the concentration container to obtain the solution to be treated. This can be achieved in the following manner: the extracted solution can be filtered through a vacuum filtration device, and the filtered solution is drained into the concentration container, and the solution placed in the concentration container is used as the solution to be treated.

[0052] It should be noted that the vacuum filtration device in this application is a glass sand core filtration device.

[0053] In some embodiments, reference Figure 2 , this figure is a structural schematic diagram of a vacuum filtration device according to some embodiments of the present application, and 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.

[0054] 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.

[0055] 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 and 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 and 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 and concentration process. Subsequently, 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 and concentration process, wherein the sampling interval is a parameter preset according to actual needs. For example, in this application, the sampling interval can be preset to 1 second.

[0056] It should be noted that the intelligent sensor in the present application is an integrated sensor that measures the temperature and volume of the solution in the concentration container and the temperature and atmospheric pressure of the external environment.

[0057] In step 103, bubble interference generated on the liquid surface of the solution to be treated during the nitrogen blowing and concentration process is identified based on 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 based on the bubble interference.

[0058] In some embodiments, identifying the bubble interference generated on the liquid surface of the solution to be treated during nitrogen purge concentration according to the fluctuation characteristics of the volume change data can be achieved by the following steps:

[0059] determining a fluctuation characteristic of the volume change data;

[0060] determining a volatilization rate sequence of the solution to be treated during nitrogen blowing and concentration according to the volume change data;

[0061] determining the abnormal interference amount in the nitrogen blowing concentration process according to the volatilization rate sequence;

[0062] The bubble interference generated on the liquid surface of the solution to be treated during the nitrogen blowing and concentration process is determined according to the abnormal interference amount and the fluctuation characteristics.

[0063] It should be noted that the fluctuation characteristic in the present application is a parameter value that measures the degree of fluctuation in the volume change of the solution to be treated during the nitrogen blowing and concentration process. The larger the fluctuation characteristic, the greater the degree of fluctuation in the volume change of the solution to be treated during the nitrogen blowing and concentration process. The smaller the fluctuation characteristic, the smaller the degree of fluctuation in 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.

[0064] In a specific implementation, determining the volatilization rate sequence of the solution to be treated during the nitrogen blowing and concentration process based on the volume change data can be achieved in the following manner: 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 using 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, using the obtained sequence as the volatilization rate sequence of the solution to be treated during the nitrogen blowing and concentration process.

[0065] It should be noted that the volatilization rate sequence in the present application is a sequence representing the change in the volatilization rate of the solvent in the solution over time during the nitrogen blowing concentration process.

[0066] 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 with the concentration rate during the nitrogen blowing concentration process. The larger the abnormal interference amount, the more interference with the concentration rate during the nitrogen blowing concentration process, and the smaller the abnormal interference amount, the less interference with 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 in the following manner, namely: the variance of the volatilization rate sequence is used as the abnormal interference amount in the nitrogen blowing concentration process.

[0067] In a specific implementation, the bubble interference generated on the liquid surface of the solution to be treated during the nitrogen blowing concentration process is determined based on the volatilization rate sequence and the fluctuation characteristics. This can be achieved in the following manner: first, the fluctuation characteristics are taken as A and the abnormal interference amount is taken as B. Subsequently, the covariance C between the sequence corresponding to the volume change data and the volatilization rate sequence is calculated. Finally, the matrix [A, C; C, B] is used as a quantization matrix of the bubble interference generated on the liquid surface of the solution to be treated during the nitrogen blowing concentration process.

[0068] It should be noted that the fluctuation characteristic in this 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.

[0069] In some embodiments, determining the loss of the solution to be treated during the nitrogen purge concentration process by using the bubble interference can be achieved by the following steps:

[0070] Determining the state vector of the solution to be processed at a current moment;

[0071] determining a plurality of state points in a state space according to the bubble interference and the state vector;

[0072] The loss amount of the solution to be treated during the nitrogen blowing and concentration process is determined according to all state points.

[0073] 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.

[0074] 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.

[0075] In specific implementation, the following method can be used to determine multiple state points in the state space based on the bubble interference and the state vector, namely: first, the quantization matrix of the bubble interference is decomposed into an upper triangular matrix and a lower triangular matrix through the Cholesky decomposition in the prior art, and then all unit basis vectors in the two-dimensional space are obtained. For each unit basis vector, the decomposed upper triangular matrix is ​​multiplied by the unit basis vector, and the obtained vector is added 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.

[0076] It should be noted that the state point in this application is the point in the state space represented by the vector that describes the state of the volume of the solution to be processed at the next moment. Since the change in the volume of the solution to be processed at the current moment is fluctuating, that is, uncertain, there are multiple situations for the state of the volume of the solution to be processed at the next moment, that is, there are multiple state points.

[0077] In a specific implementation, determining the loss amount of the solution to be treated during the nitrogen blowing and concentration process based on all state points can be achieved in the following manner: 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 and concentration process.

[0078] It should be noted that the loss amount in this application is a parameter value that measures 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 rate.

[0079] In step 104, environmental parameters collected by the intelligent sensor during the nitrogen purge concentration process are obtained, deviation characteristics of latent heat change during the nitrogen purge concentration process are determined based on the environmental parameters and the temperature change data, and a model gain of a concentration rate tracking model during the nitrogen purge concentration process is determined based on the deviation characteristics.

[0080] 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 both used as the external environmental parameters during the nitrogen blowing and concentration process.

[0081] 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.

[0082] In some embodiments, reference Figure 3 This figure is an exemplary flow chart for determining deviation characteristics according to some embodiments of the present application. In the present application, determining the deviation characteristics of the latent heat change during the nitrogen purge concentration process according to the environmental parameters and the temperature change data can be achieved by using the following steps:

[0083] In step 1041, the temperature difference at the current moment is determined according to the temperature change data;

[0084] In step 1042, a latent heat coefficient of volatilization is determined according to the environmental parameters;

[0085] In step 1043, a plurality of candidate prediction states are determined based on the latent heat coefficient of evaporation and the temperature difference at the current moment;

[0086] In step 1044 , deviation characteristics of latent heat changes during the nitrogen purge concentration process are determined based on all prediction candidate states.

[0087] It should be noted that the temperature difference in this 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 is determined according to the temperature change data in this application. It can be achieved in the following way, namely: the difference between the last two temperature values ​​in the corresponding sequence of the temperature change data is taken, and the obtained difference is used as the temperature difference at the current moment.

[0088] In specific implementation, determining the latent heat coefficient of volatilization based on 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.

[0089] It should be noted that the latent heat of volatilization coefficient in this 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.

[0090] In a specific implementation, determining multiple prediction candidate states based on the latent heat coefficient of volatility and the temperature difference at the current moment can be achieved in the following manner: first, for each state point, multiplying the time transfer matrix by the square root of 2 and then multiplying the resultant by the state point to obtain a vector Q; then, multiplying the temperature transfer matrix by the temperature difference at the current moment to obtain a vector P; then, dividing the vector P by the latent heat coefficient of volatility and then adding the resultant by the vector Q; finally, using the added vector as the prediction candidate state, thereby obtaining the prediction candidate state for 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 and concentration process.

[0091] It should be noted that the predicted candidate state in this 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.

[0092] In specific implementation, the deviation characteristics of the latent heat change during the nitrogen blowing concentration process are determined based on all the predicted candidate states. This can be achieved in the following manner: first, the average vector of all the predicted candidate states is used as the predicted concentration state of the solution to be treated. Then, for each predicted 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 resulting matrix is ​​used as a prediction deviation matrix, thereby obtaining 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.

[0093] It should be noted that the deviation characteristic in this application is a quantitative matrix that describes the change in latent heat in the solution to be treated caused by solvent volatilization during the nitrogen blowing concentration process.

[0094] In some embodiments, determining the model gain of the concentration rate tracking model during nitrogen purge concentration based on the deviation characteristics can be achieved by using the following steps:

[0095] determining a plurality of tracking points according to the deviation characteristics;

[0096] The model gain of the enrichment rate tracking model during nitrogen purge enrichment is determined based on all tracking points.

[0097] In specific implementation, determining multiple tracking points based on the deviation features can be achieved in the following manner: 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 to obtain multiple tracking points.

[0098] It should be noted that the tracking point in this 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.

[0099] In specific implementation, the model gain of the enrichment rate tracking model during the nitrogen blowing enrichment process can be determined based on all tracking points in the following manner: 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; then, the covariance matrix is ​​multiplied by the inverse matrix of the cross-covariance matrix, and the obtained value is used as the model gain.

[0100] It should be noted that the model gain in this application is a parameter used to adjust the predicted value of the concentration rate after introducing temperature uncertainty.

[0101] 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.

[0102] 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.

[0103] 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:

[0104] determining a predicted concentration rate of the solvent to be processed based on the model gain and the loss amount;

[0105] comparing the predicted concentration rate with a preset target concentration rate, and 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;

[0106] 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;

[0107] 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.

[0108] 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: 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. Subsequently, the obtained quotient is multiplied by the model gain, and the multiplied value is added to the average vector of all predicted candidate states. Finally, the second element in the vector obtained after the addition is used as the predicted concentration rate of the solvent to be treated.

[0109] It should be noted that the predicted concentration rate in this application refers to the predicted concentration rate of the solution to be treated at the next moment.

[0110] It should be noted that the target concentration rate in this 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 this application, the target concentration rate can be set to 5ml / min.

[0111] 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, that is, 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.

[0112] 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, that is, the nitrogen flow rate of the nitrogen blowing needle can be increased by 10 ml / min when the predicted concentration rate is less than the preset target concentration rate.

[0113] 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, reference Figure 4 , which is a schematic structural diagram of a nitrogen blowing and concentration processing unit according to some embodiments of the present application. The nitrogen blowing and concentration processing unit 400 includes: a collection module 401, a processing module 402 and an execution module 403, which are described as follows:

[0114] The acquisition module 401 in this 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 smart sensor to collect real-time volume change data and temperature change data of the solution to be treated during the nitrogen blowing and concentration process;

[0115] Processing module 402, in this application, is mainly used to identify bubble interference generated on the liquid surface of the solution to be treated during the nitrogen blowing concentration process based on 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 based on the bubble interference;

[0116] It should be noted that the processing module 402 in the present application is further configured to obtain environmental parameters collected by the intelligent sensor during the nitrogen purge concentration process, determine deviation characteristics of latent heat change during the nitrogen purge concentration process based on the environmental parameters and the temperature change data, and determine a model gain of a concentration rate tracking model during the nitrogen purge concentration process based on the deviation characteristics;

[0117] Execution module 403, in this 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.

[0118] In addition, the present application also provides a computer device, which includes a memory and a processor, wherein the memory stores a code, and the processor is configured to obtain the code and execute the above-mentioned nitrogen blowing concentration method for the solution.

[0119] In some embodiments, reference Figure 5 , which is a schematic diagram of the structure of a computer device for implementing the nitrogen blowing concentration method of a solution according to some embodiments of the present application. The nitrogen blowing concentration method of the solution in the above embodiment can be achieved by Figure 5 The computer device 500 shown in FIG. 5 is implemented as shown in FIG. 5 . The computer device 500 includes at least one processor 501 , a communication bus 502 , a memory 503 , and at least one communication interface 504 .

[0120] The processor 501 may be a general-purpose central processing unit (CPU) or an application-specific integrated circuit (ASIC).

[0121] The communication bus 502 may be used to transmit information between the aforementioned components.

[0122] The memory 503 may be a read-only memory (ROM) or other type of static storage device capable of storing static information and instructions, a random access memory (RAM) or other type of dynamic storage device capable of storing information and instructions, 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 compact discs, laser discs, optical discs, digital versatile discs, Blu-ray discs, etc.), a magnetic disk or other magnetic storage device, or any other medium capable of carrying or storing desired program code in the form of instructions or data structures and accessible by a computer, but is not limited thereto. The memory 503 may be independent and connected to the processor 501 via the communication bus 502. The memory 503 may also be integrated with the processor 501.

[0123] The memory 503 is used to store program code for executing the solution of the present application, and is controlled by the processor 501 for execution. 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.

[0124] The communication interface 504 uses any device such as a transceiver to communicate with other devices or communication networks, such as Ethernet, radio access network (RAN), wireless local area network (WLAN), etc.

[0125] In a specific implementation, as an example, a computer device may include multiple processors, each of which may be a single-core (single-CPU) processor or a multi-core (multi-CPU) processor. A processor herein may refer to one or more devices, circuits, and / or processing cores for processing data (e.g., computer program instructions).

[0126] The aforementioned computer device can be a general-purpose computer device or a dedicated computer device. In a specific implementation, the computer device can 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 embodiments of this application do not limit the type of computer device.

[0127] 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.

[0128] 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 the 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, 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.

[0129] 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. Subsequently, the uncertainty of temperature change (i.e., the deviation characteristics of latent heat change) is introduced to determine the model gain of the concentration rate tracking model in the nitrogen blowing concentration process, that is, the tracking model of the concentration rate of the solution to be treated is corrected when the temperature changes. Finally, the concentration rate of the solution to be treated is predicted by the loss amount and the model gain, and the nitrogen flow rate of the nitrogen blowing needle in the nitrogen blowing concentration process is adjusted 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, thereby avoiding splashing of the solution to be treated during the nitrogen blowing concentration process. In summary, the solution 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 testing.

[0130] Although the preferred embodiments of the present application have been described, those skilled in the art may make additional 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 that fall within the scope of the present application.

[0131] Obviously, those skilled in the art may make various changes and modifications to this application without departing from the spirit and scope of this application. Thus, if these modifications and variations of this application fall within the scope of the claims of this application and their equivalents, this application is intended to include these modifications and variations.

Claims

1. A method for nitrogen blowing concentration of a solution, for controlling a solvent extraction device for physical and chemical testing to carry out nitrogen blowing concentration of a solution, wherein: The solvent extraction equipment includes: a concentration container, a nitrogen valve, an intelligent sensor and a nitrogen blowing needle, and is characterized in that it includes: 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 volume change data and temperature change data of the solution to be treated during the nitrogen blowing and concentration process in real time through the intelligent sensor; Identifying 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 based on the bubble interference; obtaining environmental parameters collected by the intelligent sensor during the nitrogen purge concentration process, determining deviation characteristics of latent heat change during the nitrogen purge concentration process based on the environmental parameters and the temperature change data, and determining a model gain of a concentration rate tracking model during the nitrogen purge concentration process based on the deviation characteristics; 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, thereby completing the nitrogen blowing concentration of the solution to obtain a solution sample for physical and chemical testing; Wherein, 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 processed at a current moment; determining a plurality of state points in a state space according to the bubble interference and the state vector; Determine the loss of the solution to be treated during the nitrogen blowing and concentration process according to all state points; Among them, the concentration rate tracking model is expressed as: predicted concentration rate = [0,1]*(model gain*prediction error*loss amount+predicted concentration state), where the predicted concentration state is the average vector of all predicted candidate states, 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, and the model gain is the parameter used to adjust the predicted value of the concentration rate after introducing temperature uncertainty. The concentration rate tracking model corrects the predicted concentration state by introducing loss amount and model gain.

2. The method according to claim 1, wherein 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 a volatilization rate sequence of the solution to be treated during nitrogen blowing and concentration 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, wherein 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 candidate prediction states according to the latent heat coefficient of volatile matter and the temperature difference at a current moment; The deviation characteristics of latent heat change during nitrogen purge concentration are determined based on all prediction candidate states.

4. The method according to claim 1, wherein Adjusting the nitrogen flow rate of the nitrogen blowing needle during the nitrogen blowing concentration process according to the model gain and the loss specifically includes: determining a predicted concentration rate of the solvent to be processed based on the model gain and the loss amount; comparing the predicted concentration rate with a preset target concentration rate, and 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; 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.

5. The method according to claim 1, wherein 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.

6. The method according to claim 1, wherein Determining the model gain of the enrichment rate tracking model during the nitrogen purge 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 purge enrichment is determined based on all tracking points.

7. A solvent extraction device for physical and chemical testing, comprising a nitrogen blowing concentration unit, which adopts the method according to any one of claims 1 to 6 for nitrogen blowing concentration, characterized in that: The nitrogen blowing and concentration unit comprises: The acquisition module is used to filter the extracted solution and place it in a 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 real-time volume change data and temperature change data of the solution to be treated during the nitrogen blowing and concentration process; a processing module, configured to identify bubble interference generated on the liquid surface of the solution to be treated during the nitrogen blowing and concentration process based on the fluctuation characteristics of the volume change data, and determine the loss amount of the solution to be treated during the nitrogen blowing and concentration process based on the bubble interference; The processing module is further configured to obtain environmental parameters collected by the intelligent sensor during the nitrogen purge concentration process, determine deviation characteristics of latent heat change during the nitrogen purge concentration process based on the environmental parameters and the temperature change data, and determine a model gain of a concentration rate tracking model during the nitrogen purge 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.

8. A computer device, characterized in that: The computer device includes 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 6.

9. A computer-readable storage medium storing a computer program, characterized in that: When the computer program is executed by a processor, the nitrogen blowing concentration method for a solution according to any one of claims 1 to 6 is implemented.

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