A chromatography column separation and purification system and its application

Abstract

The present invention relates to the technical field of separation and purification, and discloses a chromatography column separation and purification system and its application, the system comprising: each group of separation and purification units comprises: a liquid storage tank, a three-way piston, a valve, a chromatography column, a flow rate management unit and a liquid collection bottle; the liquid storage tank, the three-way piston and the valve are connected in sequence, a sealing rubber plug is arranged on the top of the chromatography column, a peristaltic chamber, a peristaltic pump, a flow sensor and a processing and calculation module matching the number of the separation and purification units are arranged in the flow rate management unit, the flow rate of the solution in the peristaltic chamber is controlled by the peristaltic pump, the peristaltic chamber is connected to the liquid collection bottle through a rubber tube, and each peristaltic chamber is provided with the flow sensor. The present invention improves the efficiency and effect of separation through precise flow rate control and automated processing and calculation modules.

Description

Technical Field

[0001] The invention relates to the technical field of separation and purification, and in particular to a chromatography column separation and purification system and application thereof. Background Art

[0002] At present, the separation methods of Sr-Y include solution extraction, extraction chromatography and precipitation. The extraction method is complicated to operate, and the third phase is easily formed during solution extraction. The separation efficiency and purity of 90Y using crown ether resin extraction chromatography are difficult to guarantee. The precipitation method will introduce a large number of other co-precipitated metal ions, which limits its practical application.

[0003] The di-(2-ethylhexyl) phosphoric acid extraction chromatography method in HJ 815-2016 is suitable for the determination of 90Sr in water and animal and plant ash. After the sample to be tested is pretreated and the acidity is adjusted, its solution passes through a polychlorotrifluoroethylene (referred to as kel-F) chromatography column coated with di-(2-ethylhexyl) phosphoric acid (referred to as HDEHP) to adsorb yttrium, and then the chromatography column is eluted with 1.5mol / L nitric acid to elute other adsorbed strontium, cesium, cerium, promethium and other ions, and yttrium is desorbed with 6mol / L nitric acid, and β counting and weighing are performed in the form of yttrium oxalate precipitation. In the preparation of the HDEHP-kel-F chromatography column, the loading of the sample solution, multiple elutions to remove impurities, and the final desorption of 90Y, it is necessary to control a constant flow rate and adjust different flow rates at different steps. In previous operations, the flow rate was estimated by eye and the valve of the extraction column was manually adjusted to control the flow rate of the solution. This was time-consuming and difficult to quickly and accurately determine a constant flow rate, making it difficult to achieve simultaneous separation and purification of multiple samples. Summary of the invention

[0004] In view of this, the present invention proposes a chromatography column separation and purification system and its application, aiming to solve the problem that it is difficult to quickly and accurately determine a constant flow rate and difficult to achieve simultaneous separation and purification of multiple samples in the current technology.

[0005] A chromatography column separation and purification system proposed in the present invention comprises: a plurality of separation and purification units;

[0006] Each group of separation and purification units comprises: a liquid storage tank for storing sample solutions or eluents of different concentrations, a three-way piston for controlling the start and stop of solution injection, a valve for adjusting the solution injection speed, a chromatographic column for separating and purifying target metal ions, a flow rate management unit for controlling the solution flow rate of each group of the separation and purification units, and a liquid collection bottle; the liquid storage tank, the three-way piston and the valve are connected in sequence, a sealing rubber plug is provided on the top of the chromatographic column, and the flow rate management unit is provided with peristaltic chambers, peristaltic pumps, flow sensors and processing and calculation modules matching the number of the separation and purification units, the solution flow rate in the peristaltic chamber is controlled by the peristaltic pump, the peristaltic chamber is connected to the liquid collection bottle through a rubber tube, and each peristaltic chamber is provided with the flow sensor;

[0007] The flow rate management unit is configured to set the initial flow rates for sample loading, elution and desorption respectively, and record them as the first initial flow rate, the second initial flow rate and the third initial flow rate respectively; the flow sensor obtains the flow data and transmits it to the processing and calculation module, the processing and calculation module obtains the real-time flow rates for sample loading, elution and desorption according to the flow data and time calculation, and records them as the first real-time flow rate, the second real-time flow rate and the third real-time flow rate respectively, calculates according to each of the real-time flow rates and the corresponding initial flow rate, obtains each flow rate deviation value, and the processing and calculation module adjusts each of the real-time flow rates through the peristaltic pump according to the flow rate deviation value.

[0008] Furthermore, each of the flow velocity deviation values ​​is obtained by the following methods:

[0009] Using the difference between the first initial flow rate and the first real-time flow rate as a first flow rate deviation value, using the difference between the second initial flow rate and the second real-time flow rate as a second flow rate deviation value, and using the difference between the third initial flow rate and the third real-time flow rate as a third flow rate deviation value;

[0010] After each flow velocity deviation value is obtained, a flow velocity-time curve is established according to the acquisition time of each flow velocity deviation value.

[0011] Furthermore, before the processing and calculation module adjusts each of the real-time flow rates through the peristaltic pump according to the flow rate deviation value, it also includes:

[0012] The flow rate management unit is pre-set with the duration of each stage of sample loading, eluting and desorption, and starts timing when the sample loading process begins. The flow rate management unit determines the stage of the separation and purification process according to the duration of the sample loading, eluting and desorption and the time after the timing starts; when in the sample loading stage, the processing and calculation module adjusts the real-time flow rate according to the first flow rate deviation value; when in the eluting stage, the processing and calculation module adjusts the real-time flow rate according to the second flow rate deviation value; when in the desorption process, the processing and calculation module adjusts the real-time flow rate according to the third flow rate deviation value.

[0013] Further, when the processing and calculation module adjusts each of the real-time flow rates through the peristaltic pump according to the flow rate deviation value, it includes:

[0014] The processing and calculation module uses ±5-10% of each of the initial flow rates as a deviation threshold, and when the flow rate deviation value is within the range of the deviation threshold, determines whether the flow rate deviation value is a positive number;

[0015] When the flow rate deviation value is a positive number, the power of the peristaltic pump satisfies the following relationship:

[0016]

[0017] When the flow rate deviation value is a negative number, the power of the peristaltic pump satisfies the following relationship:

[0018]

[0019] Wherein, P is the adjusted power of the peristaltic pump, P0 is the initial power of the peristaltic pump, and δ is the percentage of the flow rate deviation value to the initial flow rate.

[0020] Further, when the processing and calculation module adjusts each of the real-time flow rates through the peristaltic pump according to the flow rate deviation value, it also includes:

[0021] When the flow velocity deviation value is not within the range of the deviation threshold, determining whether the flow velocity deviation value is a positive number;

[0022] When the flow rate deviation value is a positive number, the power of the peristaltic pump satisfies the following relationship:

[0023] P=P0+k×(ΔV-ΔV threshold );

[0024] When the flow rate deviation value is a positive number, the power of the peristaltic pump satisfies the following relationship:

[0025] P=P0-k×(ΔV-ΔV threshold);

[0026] Wherein, P is the adjusted power of the peristaltic pump, P0 is the initial power of the peristaltic pump, k is the adjustment coefficient, ΔV is the flow rate deviation value, ΔV threshold is the deviation threshold.

[0027] Further, when the flow rate deviation value is not within the range of the deviation threshold, the detection interval of the real-time flow rate is adjusted:

[0028] Obtain a flow velocity-time curve and a minimum detection interval and a maximum detection interval of the flow sensor, calculate a deviation change rate according to the flow velocity-time curve, and adjust the detection interval according to the following relationship:

[0029]

[0030] in, is the rate of change of deviation, Δt new is the adjusted detection interval, max(a,b) means taking the larger value of a and b, min(c,d) means taking the smaller value of c and d, T high Indicates the high rate of change threshold, T high The value is 5%, T low Represents the low rate of change threshold, T low The value is 2%.

[0031] Furthermore, the deviation change rate satisfies the following relationship:

[0032]

[0033] in, Indicates the rate of change of deviation, ΔV n Indicates the velocity deviation value detected for the nth time, ΔV n-1 It represents the flow velocity deviation value detected for the (n-1)th time, where n is a positive integer and n≥2.

[0034] Furthermore, the processing and calculation module is also configured to: when the deviation change rate is greater than or equal to 10%, control the valve to close and issue a warning alarm.

[0035] On the other hand, the present invention also provides an application of the above-mentioned chromatography column separation and purification system in separating strontium and yttrium. When separating strontium and yttrium, a mixture of one or more of hydrochloric acid, acetic acid and nitric acid is used as an eluent, and dimethylnitrosamine or triethanolamine is added to the eluent to separate strontium and yttrium.

[0036] Furthermore, when strontium and yttrium are separated, the column temperature of the chromatography column is 25-50°C.

[0037] Compared with the prior art, the beneficial effect of the present invention is that through precise flow rate control, efficient separation of strontium and yttrium is achieved. Traditional methods such as solution extraction and precipitation methods often face problems such as low separation efficiency and impurity interference, while the present system can provide higher separation efficiency and purity under the same conditions. The system supports the use of a variety of eluents (such as hydrochloric acid, acetic acid, nitric acid, etc.), providing flexibility for the separation of different types of samples, thereby optimizing the separation effect. The flow rate is monitored in real time by the flow sensor, and the processing and calculation module is dynamically adjusted according to the deviation between the real-time flow data and the set flow rate to ensure that the optimal flow rate is always maintained throughout the separation process. The traditional operation method relies on manual adjustment of the flow rate, which is prone to errors. The system realizes fully automatic flow rate control, significantly reduces human errors, and improves the reliability of operation. The flow sensor can obtain flow rate data in real time, and the processing and calculation module calculates the deviation value based on the preset initial flow rate and the real-time flow rate. This mechanism ensures that the flow rate is always within the set range during the separation process, ensuring the accuracy of the experimental data. When the flow rate deviation exceeds the set threshold, the system will issue an early warning in time to prompt the operator to adjust the parameters to prevent possible experimental errors. The system automatically switches the flow rate adjustment strategy according to the time settings of the three stages of sample loading, elution and desorption. This flow rate management for different stages helps to improve the overall separation efficiency and ensure that the processing at each stage achieves the best effect. The system can record the changing trend of flow rate deviation, establish a flow rate-time curve, and help analyze the dynamic changes in the separation process. This data support will provide a basis for subsequent optimization and help to continuously improve the separation process. The system can process multiple samples at the same time, saving the manpower and time costs of the laboratory. Through the automated process, the work efficiency is improved and the time required for a single experiment is reduced. Due to the accuracy of flow rate control, the amount of eluent can be effectively reduced, the experimental cost can be reduced, and the resource utilization rate can be improved. Through system monitoring and feedback, the safety of operation is improved and the safety hazards caused by human factors are reduced. Real-time monitoring and automatic adjustment mechanism ensure the stability and reliability of the separation process and reduce the probability of emergencies. The system allows the column temperature of the chromatographic column to be adjusted in the range of 25-50℃ to meet the needs of different chemical reactions. BRIEF DESCRIPTION OF THE DRAWINGS

[0038] Various other advantages and benefits will become apparent to those of ordinary skill in the art by reading the detailed description of the preferred embodiments below. The accompanying drawings are only for the purpose of illustrating the preferred embodiments and are not to be considered as limiting the present invention. Moreover, the same reference symbols are used throughout the accompanying drawings to represent the same components. In the accompanying drawings:

[0039] Figure 1 Schematic diagram of a chromatography column separation and purification system according to an embodiment of the present invention.

[0040] In the figure, 1. liquid storage tank; 2. three-way piston; 3. valve; 4. chromatography column; 41. sealing rubber plug; 5. flow rate management unit; 51. peristaltic chamber; 6. liquid collection bottle. DETAILED DESCRIPTION

[0041] Exemplary embodiments of the present disclosure will be described in more detail below with reference to the accompanying drawings. Although exemplary embodiments of the present disclosure are shown in the accompanying drawings, it should be understood that the present disclosure can be implemented in various forms and should not be limited by the embodiments described herein. On the contrary, these embodiments are provided in order to enable a more thorough understanding of the present disclosure and to fully convey the scope of the present disclosure to those skilled in the art. It should be noted that, in the absence of conflict, the embodiments of the present invention and the features described in the embodiments can be combined with each other. The present invention will be described in detail below with reference to the accompanying drawings and in combination with the embodiments.

[0042] See also Figure 1 As shown, an embodiment of the present invention provides a chromatography column separation and purification system, comprising: four groups of separation and purification units;

[0043] Each group of separation and purification units comprises: a liquid storage tank 1 for storing sample solutions or eluents of different concentrations, a three-way piston 2 for controlling the start and stop of solution injection, a valve 3 for adjusting the solution injection speed, a chromatographic column 4 for separating and purifying target metal ions, a flow rate management unit 5 for controlling the solution flow rate of each group of separation and purification units, and a liquid collecting bottle 6; the liquid storage tank 1, the three-way piston 2 and the valve 3 are connected in sequence, a sealing rubber plug 41 is provided on the top of the chromatographic column 4, and a peristaltic chamber 51, a peristaltic pump, a flow sensor and a processing and calculation module matching the number of separation and purification units are provided in the flow rate management unit 5, the solution flow rate in the peristaltic chamber 51 is controlled by the peristaltic pump, the peristaltic chamber 51 is connected to the liquid collecting bottle 6 through a rubber tube, and each peristaltic chamber 51 is provided with a flow sensor;

[0044] The flow rate management unit 5 is configured to set the initial flow rates for sample loading, elution and desorption respectively, and record them as the first initial flow rate, the second initial flow rate and the third initial flow rate respectively; the flow sensor obtains the flow data and transmits it to the processing and calculation module, the processing and calculation module obtains the real-time flow rate of sample loading, elution and desorption according to the flow data and time calculation, and records them as the first real-time flow rate, the second real-time flow rate and the third real-time flow rate respectively, calculates according to each real-time flow rate and the corresponding initial flow rate, obtains each flow rate deviation value, and the processing and calculation module adjusts each real-time flow rate through the peristaltic pump according to the flow rate deviation value.

[0045] It should be noted that the liquid storage tank 1 is used to store sample solutions or eluents of different concentrations, supports the storage and transportation of multiple liquids, effectively prevents leakage and contamination of liquids, and ensures the purity and stability of the solution during the experiment. The three-way piston 2 is used to manually control the start and stop of solution injection, so that the system can accurately control the flow time and flow rate of the liquid. The valve 3 is used to adjust the injection speed so that the flow rate can be accurately adjusted according to the experimental requirements, thereby ensuring that the solution flow rate during the entire separation process meets the preset value. The three-way piston 2 and the valve 3 can seal the chromatographic column 4, which is conducive to the long-term preservation of the sample. The material of the valve 3 is a material with strong corrosion resistance, which can effectively extend the service life of the equipment. The chromatographic column 4 is used to separate and purify the target metal ions. The filling material in the column can be selectively replaced according to the experimental requirements to improve the separation efficiency and purity. The sealing rubber plug 41 at the top of the chromatographic column 4 ensures that the solution remains sealed when flowing through the chromatographic column 4, avoiding interference from external air and impurities, thereby improving the separation purity and the reliability of the experimental results. The flow rate management unit 5 has a built-in peristaltic chamber 51, a peristaltic pump, a flow sensor and a processing and calculation module, which realizes precise control of the solution flow rate. By dynamically adjusting the flow rate, the unit can automatically maintain the preset flow rate value, thereby ensuring that the flow rate in the sample loading, elution and desorption stages is always within the optimal range. The flow sensor monitors the solution flow rate in real time and transmits the data to the processing and calculation module. The module calculates the flow rate deviation value based on the acquired data, and adjusts the flow rate in time through the peristaltic pump to ensure the accuracy and stability of the separation process. The liquid collection bottle 6 is used to collect the liquid treated by the chromatographic column 4 to ensure that no secondary pollution occurs during the operation of the entire system. Its design ensures that the collected liquid will not leak, thereby maintaining the cleanliness and safety of the experimental environment. The material of the liquid collection bottle 6 is transparent, which is convenient for observing the collection of liquid during the experiment. When the liquid is collected, the bottle can be quickly replaced, thereby improving the convenience of experimental operation.

[0046] In some embodiments of the present application, each flow rate deviation value is obtained by the following method:

[0047] The difference between the first initial flow rate and the first real-time flow rate is used as the first flow rate deviation value, the difference between the second initial flow rate and the second real-time flow rate is used as the second flow rate deviation value, and the difference between the third initial flow rate and the third real-time flow rate is used as the third flow rate deviation value;

[0048] After each flow velocity deviation value is obtained, a flow velocity-time curve is established according to the acquisition time of each flow velocity deviation value.

[0049] It can be understood that the definition and acquisition of flow rate deviation value is:

[0050] In this system, the control of solution flow rate is divided into three stages: sample loading stage, elution stage and desorption stage. For each stage, the system pre-sets an initial flow rate, namely:

[0051] First initial flow rate: target flow rate when loading the sample. Second initial flow rate: target flow rate when eluting. Third initial flow rate: target flow rate when desorbing.

[0052] During actual operation, the system monitors the flow rate in real time and obtains real-time flow rate data:

[0053] First real-time flow rate: the current flow rate detected by the system during sample loading. Second real-time flow rate: the current flow rate detected by the system during elution. Third real-time flow rate: the current flow rate detected by the system during desorption. By comparing the initial flow rate of each stage with the corresponding real-time flow rate, the flow rate deviation value of each stage can be calculated: first flow rate deviation value = first initial flow rate - first real-time flow rate; second flow rate deviation value = second initial flow rate - second real-time flow rate; third flow rate deviation value = third initial flow rate - third real-time flow rate. These deviation values ​​reflect the gap between the actual flow rate and the target flow rate, and are important indicators for evaluating the accuracy of flow rate control.

[0054] Establish a flow rate-time curve based on the flow rate deviation value

[0055] During the operation of the system, the flow sensor will continuously detect the flow rate of the solution and record this data in the processing and calculation module, while also recording the time when the data was acquired.

[0056] After obtaining the flow rate deviation value at each stage, the system pairs each deviation value with its corresponding time point to establish a flow rate-time curve.

[0057] Flow rate-time curve

[0058] This curve shows the change in solution flow rate during the entire experiment. It uses time as the horizontal axis (X-axis) and flow rate or flow rate deviation value as the vertical axis (Y-axis), reflecting the fluctuation of flow rate at different time points. By observing the flow rate-time curve, it can be found whether the flow rate is within the stable range, and whether there are abnormal flow rates at certain specific time points, so as to make real-time adjustments to the system. The purpose of establishing this curve is to display the flow rate change trend in a visual way, and to assist the system in further flow rate regulation to ensure that the flow rate at each stage is within the expected range, thereby improving the efficiency and stability of the separation and purification process.

[0059] By obtaining the flow rate deviation value and establishing the flow rate-time curve, the system can monitor and feedback the changes in the solution flow rate in real time to ensure that the flow rate always meets the experimental requirements. If the curve shows a large flow rate deviation, the system can make instant adjustments through the peristaltic pump to control the flow rate deviation within the allowable range, thereby improving the efficiency of separation and purification. The flow rate-time curve is not only used for real-time control, but also for subsequent data analysis and experimental optimization. Experimenters can further improve the performance of the system by analyzing the curve, improving the initial flow rate setting or optimizing the system structure.

[0060] In some embodiments of the present application, before the processing and calculation module adjusts each real-time flow rate through the peristaltic pump according to the flow rate deviation value, it also includes:

[0061] The flow rate management unit 5 is pre-set with the duration of each stage of sample loading, eluting and desorption, and starts timing when the sample loading process begins. The flow rate management unit 5 determines the stage of the separation and purification process according to the duration of sample loading, eluting and desorption and the time after the timing starts; when in the sample loading stage, the processing and calculation module adjusts the real-time flow rate according to the first flow rate deviation value; when in the eluting stage, the processing and calculation module adjusts the real-time flow rate according to the second flow rate deviation value; when in the desorption process, the processing and calculation module adjusts the real-time flow rate according to the third flow rate deviation value.

[0062] In some embodiments of the present application, when the processing and calculation module adjusts each real-time flow rate through a peristaltic pump according to the flow rate deviation value, it includes:

[0063] The processing and calculation module uses ±5-10% of each initial flow rate as a deviation threshold, and when the flow rate deviation value is within the range of the deviation threshold, determines whether the flow rate deviation value is a positive number;

[0064] When the flow rate deviation value is positive, the power of the peristaltic pump satisfies the following relationship:

[0065]

[0066] When the flow rate deviation value is negative, the power of the peristaltic pump satisfies the following relationship:

[0067]

[0068] Wherein, P is the adjusted peristaltic pump power, P0 is the initial power of the peristaltic pump, and δ is the percentage of the flow rate deviation value to the initial flow rate.

[0069] In some embodiments of the present application, when the processing and calculation module adjusts each real-time flow rate through a peristaltic pump according to the flow rate deviation value, it also includes:

[0070] When the flow rate deviation value is not within the range of the deviation threshold, determining whether the flow rate deviation value is a positive number;

[0071] When the flow rate deviation value is positive, the power of the peristaltic pump satisfies the following relationship:

[0072] P=P0+k×(ΔV-ΔV threshold );

[0073] When the flow rate deviation value is positive, the power of the peristaltic pump satisfies the following relationship:

[0074] P=P0-k×(ΔV-ΔV threshold );

[0075] Where P is the adjusted peristaltic pump power, P0 is the initial power of the peristaltic pump, k is the adjustment coefficient, ΔV is the flow rate deviation value, ΔV threshold is the deviation threshold.

[0076] It should be noted that the method for determining the adjustment coefficient k is:

[0077] 1. Experimental Preparation

[0078] System initialization: Prepare the separation and purification system of the chromatography column 4, and ensure that the liquid storage tank 1, three-way piston 2, valve 3, flow sensor, peristaltic pump and other components are in normal working condition. Use the standard sample solution and set the initial conditions of the chromatography column 4, such as solution concentration, solution volume, column pressure, etc., to ensure that all variables remain consistent.

[0079] Initial flow rate setting: Set the initial flow rates (first initial flow rate, second initial flow rate and third initial flow rate) for sample loading, elution and desorption processes, and record these initial values.

[0080] 2. Experimental testing and data recording

[0081] Flow rate test: Before starting the test, record the current system temperature, ambient temperature and other external conditions to ensure that subsequent tests are performed in the same environment.

[0082] The sample loading, elution and desorption processes are carried out in sequence. After each process starts, the real-time flow rate value (first real-time flow rate, second real-time flow rate, third real-time flow rate) read by the flow sensor is recorded.

[0083] The real-time flow velocity value is compared with the corresponding initial flow velocity value, and the flow velocity deviation value at each stage is calculated.

[0084] Flow rate change record:

[0085] In the flow rate test of each stage, the flow rate data is recorded at fixed time intervals (such as every 5 seconds), and the data of the entire stage is continuously recorded until the process is completed.

[0086] Plot the flow rate versus time curve to observe the trend of the deviation value.

[0087] 3. Calculation of adjustment coefficient k

[0088] For the flow rate deviation value, a proportional regulation mode can be used, that is, the regulation strength of the peristaltic pump is determined by the deviation between the real-time flow rate and the initial flow rate. Set k as the regulation coefficient of the deviation value, and the formula is as follows: ΔP = k × deviation value, where ΔP represents the regulation power increment of the peristaltic pump.

[0089] Select an initial k value (such as 0.1) and test the sample loading, elution and desorption processes.

[0090] Observe the response effect of system flow rate regulation under this k value:

[0091] If the flow rate can quickly stabilize near the set value without obvious oscillation or overshoot, record the k value as the current adjustment coefficient. If the flow rate is adjusted too slowly, increase the k value appropriately (for example, increase k to 0.2 or greater) and retest. If the system has obvious oscillation or overshoot during the adjustment process, reduce the k value (for example, reduce k to 0.05) and retest.

[0092] Iterative Adjustment:

[0093] Adjust the k value repeatedly until you find a k value that responds quickly but has no obvious oscillation or overshoot.

[0094] The k value finally determined should make the real-time flow rate of each stage tend to be stable within a set time (such as within 5 seconds), and the deviation value is within an acceptable range (such as ±5% of the initial flow rate).

[0095] 4. Verification and Optimization of Adjustment Coefficient

[0096] Repeat the test:

[0097] After the initial k value is determined, multiple cycle tests are repeated, including different batches of sample loading, elution and desorption processes, to verify the applicability and stability of this k value.

[0098] Environmental Conditions Verification:

[0099] Verify under different ambient temperatures and system states to ensure the robustness of the k value under various conditions. If the effect is not ideal under other environmental conditions, the k value can be slightly adjusted.

[0100] In some embodiments of the present application, when the flow rate deviation value is not within the range of the deviation threshold, the detection interval of the real-time flow rate is adjusted:

[0101] Obtain the flow velocity-time curve and the minimum detection interval and maximum detection interval of the flow sensor, calculate the deviation change rate according to the flow velocity-time curve, and adjust the detection interval according to the following relationship:

[0102]

[0103] Where φ is the rate of change of deviation, Δt new is the adjusted detection interval, max(a,b) means taking the larger value of a and b, min(c,d) means taking the smaller value of c and d, T high Indicates the high rate of change threshold, T high The value is 5%, T low Represents the low rate of change threshold, T low The value is 2%.

[0104] It should be noted that by setting the deviation value of the initial flow rate and the real-time flow rate, and dynamically adjusting the power of the peristaltic pump when the deviation value exceeds the preset range, high-precision control of the flow rate can be achieved. Whether in the loading, elution or desorption stage, the stability of the flow rate can be guaranteed, thereby improving the efficiency and accuracy of the separation and purification process. The system automatically adjusts the power of the peristaltic pump according to the flow rate deviation value, without manual intervention, simplifying the operation process. In addition, the processing and calculation module dynamically adjusts the real-time detection interval by calculating the flow rate deviation value and the flow rate-time curve, realizes the adaptive optimization of the system, and further improves the flexibility and stability of the flow rate regulation. By accurately controlling the flow rate of each stage, it is ensured that the flow rate during sample loading, elution and desorption is kept within the optimal range, thereby effectively improving the efficiency of separation and purification, reducing the consumption of solvent and time, and enhancing the separation and purification effect of the system. By setting ±5-10% of the initial flow rate as the deviation threshold, the sensitivity of the system can be flexibly adjusted according to different experimental requirements. The range setting of the deviation threshold enables the system to automatically adjust the power of the pump when the flow rate fluctuates slightly, thereby maintaining the stability of the flow rate and avoiding fluctuations caused by over-regulation. When the deviation value is not within the deviation threshold range, the system can respond quickly and adjust the pump power, and automatically adjust the detection frequency according to the flow rate change rate. This design allows the system to quickly correct flow rate anomalies in a short period of time, ensuring the stability and continuity of the flow rate during the experiment. The system reduces the reliance on manual operation during the experiment and reduces the risk of human error through automated flow rate detection and adjustment functions. At the same time, the system's adaptive adjustment and real-time monitoring functions enable it to maintain high stability during long-term operation, improving the reliability and efficiency of the system.

[0105] In some embodiments of the present application, the deviation change rate satisfies the following relationship:

[0106]

[0107] in, Indicates the rate of change of deviation, ΔV n Indicates the velocity deviation value detected for the nth time, ΔV n-1 It represents the flow velocity deviation value detected for the (n-1)th time, where n is a positive integer and n≥2.

[0108] In some embodiments of the present application, the processing and calculation module is further configured to: when the deviation change rate is greater than or equal to 10%, control the valve 3 to close and issue a warning alarm.

[0109] In addition, this embodiment also provides an application of the separation and purification system based on the above-mentioned chromatographic column 4 in separating strontium and yttrium. Specifically, when separating strontium and yttrium, a mixture of one or more of hydrochloric acid, acetic acid and nitric acid is used as an eluent, and dimethylnitrosamine or triethanolamine is added to the eluent to separate strontium and yttrium.

[0110] Preferably, when separating strontium and yttrium, the column temperature of the chromatography column 4 is 25-50°C.

[0111] It should be noted that by calculating the change rate of the flow rate deviation, when the change rate is greater than or equal to 10%, the system can automatically close valve 3 and sound an alarm. This mechanism effectively prevents the flow rate from being out of control in the event of system failure or abnormality, ensures the safety of the experiment and the continuity of the separation and purification process, and improves the reliability and stability of the system.

[0112] By using a mixture of hydrochloric acid, acetic acid and nitric acid as the eluent and adding dimethylnitrosamine or triethanolamine, strontium and yttrium can be separated efficiently. This combination of eluents improves the selectivity and efficiency of the separation process, ensuring the purification effect of strontium and yttrium. In addition, a variety of eluent options are provided, allowing users to flexibly choose the appropriate combination according to actual needs.

[0113] The column temperature of the chromatographic column 4 is controlled (preferably in the range of 25-50° C.) to ensure that the temperature is stable and within a suitable range during the separation of strontium and yttrium. Accurate temperature control helps to improve the separation efficiency and avoid the reduction of the separation effect due to temperature fluctuations.

[0114] The system's processing and calculation module can monitor flow rate deviation in real time and take countermeasures when the deviation change rate exceeds the set value. This makes the system highly sensitive and responsive, thereby ensuring precise control of flow rate during the separation process and effectively improving separation effect and efficiency.

[0115] By preferentially using specific eluents and additives (such as dimethylnitrosamine or triethanolamine), the system can reduce the amount of chemical reagents used while ensuring the separation effect, thereby achieving the goals of efficient separation and cost control.

[0116] The system can adjust the composition of the eluent and the temperature of the chromatographic column 4 according to different separation tasks, making it highly versatile and suitable for separating different types of metal ions. This flexibility enables the system to maintain an efficient and stable working state under a variety of experimental conditions, making it more adaptable.

[0117] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention rather than to limit it. Although the present invention has been described in detail with reference to the above embodiments, ordinary technicians in the relevant field should understand that the specific implementation methods of the present invention can still be modified or replaced by equivalents. Any modification or equivalent replacement that does not depart from the spirit and scope of the present invention should be covered within the scope of protection of the claims of the present invention.

Claims

1. A chromatography column separation and purification system, characterized in that: include: Several groups of separation and purification units; Each group of separation and purification units comprises: a liquid storage tank for storing sample solutions or eluents of different concentrations, a three-way piston for controlling the start and stop of solution injection, a valve for adjusting the solution injection speed, a chromatographic column for separating and purifying target metal ions, a flow rate management unit for controlling the solution flow rate of each group of the separation and purification units, and a liquid collection bottle; the liquid storage tank, the three-way piston and the valve are connected in sequence, a sealing rubber plug is provided on the top of the chromatographic column, and the flow rate management unit is provided with peristaltic chambers, peristaltic pumps, flow sensors and processing and calculation modules matching the number of the separation and purification units, the solution flow rate in the peristaltic chamber is controlled by the peristaltic pump, the peristaltic chamber is connected to the liquid collection bottle through a rubber tube, and each peristaltic chamber is provided with the flow sensor; The flow rate management unit is configured to set the initial flow rates for sample loading, elution and desorption respectively, and record them as the first initial flow rate, the second initial flow rate and the third initial flow rate respectively; the flow sensor obtains the flow data and transmits it to the processing and calculation module, the processing and calculation module obtains the real-time flow rates for sample loading, elution and desorption according to the flow data and time calculation, and records them as the first real-time flow rate, the second real-time flow rate and the third real-time flow rate respectively, calculates according to each of the real-time flow rates and the corresponding initial flow rate, obtains each flow rate deviation value, and the processing and calculation module adjusts each of the real-time flow rates through the peristaltic pump according to the flow rate deviation value.

2. A chromatography column separation and purification system according to claim 1, characterized in that: Each of the flow velocity deviation values ​​is obtained by the following methods: Using the difference between the first initial flow rate and the first real-time flow rate as a first flow rate deviation value, using the difference between the second initial flow rate and the second real-time flow rate as a second flow rate deviation value, and using the difference between the third initial flow rate and the third real-time flow rate as a third flow rate deviation value; After each flow velocity deviation value is obtained, a flow velocity-time curve is established according to the acquisition time of each flow velocity deviation value.

3. A chromatography column separation and purification system according to claim 2, characterized in that: Before the processing and calculation module adjusts each of the real-time flow rates through the peristaltic pump according to the flow rate deviation value, it also includes: The flow rate management unit is pre-set with the duration of each stage of sample loading, eluting and desorption, and starts timing when the sample loading process begins. The flow rate management unit determines the stage of the separation and purification process according to the duration of the sample loading, eluting and desorption and the time after the timing starts; when in the sample loading stage, the processing and calculation module adjusts the real-time flow rate according to the first flow rate deviation value; when in the eluting stage, the processing and calculation module adjusts the real-time flow rate according to the second flow rate deviation value; when in the desorption process, the processing and calculation module adjusts the real-time flow rate according to the third flow rate deviation value.

4. A chromatography column separation and purification system according to claim 3, characterized in that: When the processing and calculation module adjusts each of the real-time flow rates through the peristaltic pump according to the flow rate deviation value, it includes: The processing and calculation module uses ±5-10% of each of the initial flow rates as a deviation threshold, and when the flow rate deviation value is within the range of the deviation threshold, determines whether the flow rate deviation value is a positive number; When the flow rate deviation value is a positive number, the power of the peristaltic pump satisfies the following relationship: When the flow rate deviation value is a negative number, the power of the peristaltic pump satisfies the following relationship: Wherein, P is the adjusted power of the peristaltic pump, P0 is the initial power of the peristaltic pump, and δ is the percentage of the flow rate deviation value to the initial flow rate.

5. A chromatography column separation and purification system according to claim 4, characterized in that: When the processing and calculation module adjusts each of the real-time flow rates through the peristaltic pump according to the flow rate deviation value, it also includes: When the flow velocity deviation value is not within the range of the deviation threshold, determining whether the flow velocity deviation value is a positive number; When the flow rate deviation value is a positive number, the power of the peristaltic pump satisfies the following relationship: P=P0+k×(ΔV-ΔV threshold ); When the flow rate deviation value is a positive number, the power of the peristaltic pump satisfies the following relationship: P=P0-k×(ΔV-ΔV threshold ); Wherein, P is the adjusted power of the peristaltic pump, P0 is the initial power of the peristaltic pump, k is the adjustment coefficient, ΔV is the flow rate deviation value, ΔV threshold is the deviation threshold.

6. A chromatography column separation and purification system according to claim 5, characterized in that: When the flow rate deviation value is not within the range of the deviation threshold, the detection interval of the real-time flow rate is adjusted: Obtain a flow velocity-time curve and a minimum detection interval and a maximum detection interval of the flow sensor, calculate a deviation change rate according to the flow velocity-time curve, and adjust the detection interval according to the following relationship: in, is the rate of change of deviation, Δt new is the adjusted detection interval, max(a,b) means taking the larger value of a and b, min(c,d) means taking the smaller value of c and d, T high Indicates the high rate of change threshold, T high The value is 5%, T low Represents the low rate of change threshold, T low The value is 2%.

7. A chromatography column separation and purification system according to claim 6, characterized in that: The deviation change rate satisfies the following relationship: in, Indicates the rate of change of deviation, ΔV n Indicates the velocity deviation value detected for the nth time, ΔV n-1 It represents the flow velocity deviation value detected for the (n-1)th time, where n is a positive integer and n≥2.

8. A chromatography column separation and purification system according to claim 7, characterized in that: The processing and calculation module is also configured to: when the deviation change rate is greater than or equal to 10%, control the valve to close and issue a warning alarm.

9. A use of the chromatography column separation and purification system according to any one of claims 1 to 8 in separating strontium and yttrium, characterized in that: One or a mixture of hydrochloric acid, acetic acid and nitric acid is used as an eluent, and dimethylnitrosamine or triethanolamine is added to the eluent to separate strontium and yttrium.

10. Use of the chromatography column separation and purification system according to claim 9, characterized in that: When separating strontium and yttrium, the column temperature of the chromatography column is 25-50°C.

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