CN113049668B - Dynamic separation process research and analysis system and method - Google Patents
Dynamic separation process research and analysis system and method Download PDFInfo
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- CN113049668B CN113049668B CN202110208655.8A CN202110208655A CN113049668B CN 113049668 B CN113049668 B CN 113049668B CN 202110208655 A CN202110208655 A CN 202110208655A CN 113049668 B CN113049668 B CN 113049668B
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Abstract
The invention provides a dynamic separation process research and analysis system and a dynamic separation process research and analysis method, and belongs to the field of experimental analysis devices. By establishing a dynamic separation process research and analysis system constructed by the suction device, the separation device, the detection device and the liquid storage device, dynamic input and component detection are carried out on the liquid to be detected, the continuity of the experiment is improved, and the experiment efficiency is improved; meanwhile, dynamic adsorption separation, elution and component dynamic detection are carried out on the preset substances in the liquid to be detected, so that dynamic separation data of the preset substances are obtained, and accurate data reference is provided for screening out the adsorption substances with strong adsorption capacity and high adsorption efficiency. Compared with the prior art, the invention can improve the experimental efficiency; meanwhile, the experimental result is beneficial to industrial popularization and application.
Description
Technical Field
The invention belongs to the field of experimental analysis devices, and particularly relates to a dynamic separation process research and analysis system and method.
Background
In industrial applications, it is often the case that a certain substance is separated to obtain a specific substance. In order to improve the separation efficiency and verify the separation effect of different adsorption substances on the specific substances, multiple experiments are usually required to be performed on the different adsorption substances to find the adsorption substances suitable for industrial application. For example, recovery of valuable metals in electronic waste, including noble metals, copper, nickel, etc., requires separation and purification of various valuable elements by suitable separation materials and methods, including adsorption separation, ion exchange separation, etc. In the field of analytical science, separation of an analyte from a sample matrix is often a necessary means for ensuring the selectivity of an analytical method and the reliability of an analytical result, and adsorption, ion exchange, and the like are also commonly used separation methods.
In the prior art, the process of performing a separation analysis on a sample is usually static and intermittent, i.e. the component content of the separation solution is measured at selected time points to obtain experimental data of the separation analysis. For example, in the process of ion exchange separation of valuable metal elements, a batch method is generally used, a solution containing elements to be separated and recovered is fully mixed with an ion exchanger in a batch reactor, the two are separated after a certain contact time, the elements adsorbed by the ion exchanger are desorbed, and then the ion exchanger is subjected to a regeneration treatment for reuse. This method is not only time-consuming and laborious; at the same time, this method generally only verifies that the adsorbent has a high adsorption capacity, but how much the rate of adsorption is unknown. That is, by means of the prior art, an adsorbent having a strong adsorption capacity may be screened, but a low adsorption rate is obviously difficult to adapt to dynamic adsorption applications in industry. In the field of analytical science, similar batch methods are used for separating an object to be detected, and the problems of low analysis efficiency, poor analysis effect and the like exist.
Disclosure of Invention
The invention provides a dynamic separation process research and analysis system and a method, wherein the dynamic separation process research and analysis system is formed by a suction device, a separation device, a detection device and a liquid storage device, and predetermined substances in liquid to be detected are subjected to adsorption separation, elution and dynamic detection, so that dynamic separation data are obtained, and the experimental result is favorably subjected to industrial popularization and application; meanwhile, through dynamic separation analysis, the experimental efficiency can be improved, and the operation is simple.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
in a first aspect, embodiments of the present invention provide a dynamic separation process research and analysis system comprising:
suction means for sucking the liquid;
a separation device filled with a replaceable adsorption material for separating a predetermined material in the liquid output from the suction device;
the detection device is used for detecting the content of each component of the output liquid of the separation device;
the liquid storage device is at least three groups of liquid storage devices respectively used for containing cleaning liquid, eluent and liquid to be detected, and in the working state, the outlet ends of the liquid storage devices are respectively communicated with the inlet ends of the suction devices, and a first passage used for circulating the cleaning liquid to clean the system, a second passage used for circulating the liquid to be detected and adsorbing and detecting the predetermined substances therein, and a third passage used for circulating the eluent and eluting and detecting the adsorbed predetermined substances are respectively formed.
In a further embodiment, the device further comprises a first pipeline connected with the liquid storage device and the suction device, and a valve body assembly used for controlling on-off of the first pipeline is arranged on the first pipeline.
In a further embodiment, the first pipe comprises a plurality of branches connected in parallel and a manifold connected to the branches; the branch pipes are correspondingly communicated with the liquid storage device; the main pipe is communicated with the inlet end of the suction device; the valve body assembly comprises a plurality of electromagnetic valves which are arranged on the branch pipes in a one-to-one correspondence manner.
In a further embodiment, the dynamic separation analysis of the reservoir device further comprises:
the object placing table is provided with a degree of freedom for rotating around a fixed axis, a plurality of object placing grooves for placing containers are formed in the top surface of the object placing table around the direction of the rotating axis, and the containers are used for containing cleaning liquid, eluent and liquid to be detected;
the driving motor is connected with the bottom of the circular object placing table and is used for driving the circular object placing table to horizontally rotate;
the number of the first pipelines is one, and the first pipelines can be bent and extend into the container in the storage groove.
In a further embodiment, the first pipeline comprises a first hard pipe, a second hard pipe, a first hose with two ends respectively connected with the first hard pipe and the second hard pipe, and a driving device arranged on the first pipeline and used for driving the first pipeline to stretch and bend.
In a further embodiment, the driving means comprises:
the middle part of the sleeve block is provided with two through holes, and the sleeve block is sleeved on the first hard tube and the second hard tube respectively;
the two ends of the air cylinder are respectively connected with the side edges of the two sleeve blocks in a rotating way;
the motor is arranged on one of the sleeve blocks;
the gear set is connected with the motor output shaft and the air cylinder in a transmission way.
In a further embodiment, the solenoid valve is a diaphragm solenoid valve and/or a hose squeeze valve.
In a further embodiment, the suction device employs a peristaltic pump.
In a further embodiment, the dynamic separation process research and analysis system further comprises a frothing device, the frothing device being arranged between the separation device and the detection device.
In a second aspect, embodiments of the present invention also provide an analysis method of a dynamic separation process research and analysis system, comprising:
step 1: the suction device sucks the cleaning liquid, the cleaning liquid sequentially passes through the suction device and the separation device and is washed, and the detection device detects residual components in the washed liquid;
step 2: the suction device sucks liquid to be detected, the liquid to be detected sequentially passes through the suction device and the separation device, the separation device adsorbs preset substances in the liquid to be detected, the adsorbed liquid is conveyed to the detection device, and the detection device dynamically detects residual components in the adsorbed liquid;
step 3: the suction device sucks the cleaning liquid, the cleaning liquid sequentially passes through the suction device and the separation device and is washed, the washed liquid is conveyed to the detection device, and the detection device dynamically detects the content of unadsorbed components in the washed liquid;
step 4: the suction device sucks the eluent and conveys the eluent to the separation device, the eluent elutes the predetermined substances adsorbed in the separation device, the eluted liquid is conveyed to the detection device, and the detection device dynamically detects the component content in the eluted liquid;
step 5: the suction device sucks the cleaning liquid, and the cleaning liquid sequentially passes through the suction device and the separation device to wash out residual eluent.
The beneficial effects are that: the dynamic separation process research and analysis system provided by the invention can perform dynamic adsorption separation, elution and component dynamic detection on the predetermined substances in the liquid to be detected, so that dynamic separation data of the predetermined substances are obtained, accurate data reference is provided for screening out the adsorption substances with strong adsorption capacity and high adsorption efficiency, and the experimental result is favorable for industrial popularization and application. Meanwhile, the dynamic separation analysis method is simple to operate and can also greatly improve experimental efficiency.
Drawings
FIG. 1 is a schematic diagram of the dynamic separation process research and analysis system of the present invention.
Fig. 2 is a schematic structural view of a first embodiment of the present invention.
Fig. 3 is a schematic structural diagram of a second embodiment of the present invention.
Fig. 4 is a schematic structural view of a third embodiment of the present invention.
FIG. 5 is a schematic diagram of the improved structure of the dynamic separation process research and analysis system of the present invention.
Fig. 6 is a schematic structural diagram of the first pipeline and the driving device of the present invention.
Fig. 7 is a schematic structural view of the driving device of the present invention.
The everywhere marks in fig. 1 to 7 are respectively: the suction device 10, the separation device 20, the detection device 30, the conveying pipeline 40, the first pipeline 41, the first hard pipe 411, the second hard pipe 412, the first hose 413, the second pipeline 42, the third pipeline 43, the valve body assembly 50, the foaming device 60, the object placing table 70, the object placing groove 71, the driving device 80, the sleeve block 81, the air cylinder 82, the motor 83, the gear set 84, and the liquid storage device 90.
Detailed Description
The technical scheme of the invention will be clearly and completely described below with reference to the accompanying drawings and examples. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without any inventive effort, are intended to be within the scope of the invention.
In the prior art, the process of performing a separation analysis on a sample is usually static and intermittent, i.e. the component content of the separation solution is measured at selected time points to obtain experimental data of the separation analysis. This method is not only time-consuming and laborious; at the same time, this method generally only verifies that the adsorbent has a high adsorption capacity, but how much the rate of adsorption is unknown. That is, by means of the prior art, an adsorbed substance having a strong adsorption capacity but a low adsorption rate may be screened out, and it is obvious that such a substance is difficult to adapt to dynamic adsorption applications in industry.
FIG. 1 is a schematic diagram of the dynamic separation process research and analysis system provided by the present invention. As shown in fig. 1, the dynamic separation process research and analysis system provided by the present invention includes: the suction device 10, the separation device 20, the detection device 30, and the liquid storage device 90.
The liquid storage device 90 includes at least three groups for respectively containing a cleaning liquid, an eluent and a liquid to be detected. A common cleaning fluid is clean water. The suction device 10 is used to suck liquid from a liquid storage device. The separation device 20 is filled with an exchangeable adsorption material, by which a predetermined substance in the liquid supplied to the separation device by the suction device can be separated. The detection device 30 is used for detecting the content of each component of the output liquid of the separation device. In an operating state, the outlet ends of the liquid storage devices 90 are respectively connected to the inlet ends of the suction devices 10, and form first passages for circulating a cleaning liquid to clean the system, second passages for circulating a liquid to be detected and adsorbing and detecting a predetermined substance therein, and third passages for circulating an eluent and eluting and detecting the adsorbed predetermined substance. In the present application, in order to realize the above-described passage, the communication relationship among the liquid storage device 90, the suction device 10, the separation device 20, and the detection device 30 is established by the delivery pipe 40. The conveying pipeline 40 specifically includes a first pipeline 41, a second pipeline 42, and a third pipeline 43. The connection of the suction device 10, the separating device 20 and the detecting device 30 is established via the supply line 40. Specifically, the first line 41, the suction device 10, the second line 42, the separation device 20, the third line 43, and the detection device 30 are connected in series in this order. Meanwhile, the first pipeline 41 is also provided with a valve body assembly 50. The switching of the passage is realized by controlling the on-off of the first pipeline 41 through the valve body assembly 50. When the first passage is communicated, the second passage and the third passage are closed, only the flushing liquid is supplied, and the liquid to be detected and the eluent are not supplied. When the second passage is communicated, the first passage and the third passage are closed, only the liquid to be detected is supplied, and no flushing liquid and no eluent are supplied. When the third passage is communicated, the first passage and the second passage are closed, only the eluent is supplied, and the flushing liquid and the liquid to be detected are not supplied.
In one possible embodiment, the first line 41 comprises a plurality of branches connected in parallel and a manifold connected to the branches. Each of the branch pipes is respectively communicated with each group of liquid storage devices 90 for containing different liquids. And the manifold communicates with the inlet end of the suction device 10 to direct the liquid in each of the sub-tubes to the suction device 10. The valve body assembly 50 comprises a plurality of electromagnetic valves, and the electromagnetic valves are arranged in one-to-one correspondence with the branch pipes, namely, each branch pipe is provided with an electromagnetic valve for controlling the on-off of the branch pipe. The electromagnetic valve can adopt a diaphragm electromagnetic valve or a hose squeezing valve or can adopt the condition that two valve bodies are shared. The diaphragm solenoid valve may be a two-position two-way valve or a two-position three-way valve, and the hose squeeze valve may be a single, double, or multiple valve.
In use, the end of each of the branch pipes remote from the suction device 10 extends into a liquid storage device 90 for containing liquid, wherein the containers respectively hold flushing liquid, liquid to be detected and eluent. When the sample needs to be separated and analyzed, firstly, the flushing liquid is sucked by the suction device 10, sequentially passes through the suction device 10 and the separation device 20 through the conveying pipeline 40, and the detection device 30 detects the residual components in the flushed liquid; in the process, only the electromagnetic valve on the branch pipe corresponding to the flushing liquid is opened, and other electromagnetic valves are closed. Secondly, the suction device 10 sucks liquid to be detected, the liquid to be detected sequentially passes through the suction device 10 and the separation device 20 through the conveying pipeline 40, the separation device 20 adsorbs specified components in the liquid to be detected, the adsorbed liquid is conveyed to the detection device 30, and the detection device 30 dynamically detects residual components in the adsorbed liquid; in the process, only the electromagnetic valve on the branch pipe corresponding to the liquid to be detected is opened, and other electromagnetic valves are closed. Then, the suction device 10 sucks the flushing liquid again, the flushing liquid sequentially passes through the suction device 10 and the separation device 20 through the conveying pipeline 40, the flushed liquid is conveyed to the detection device 30, and the detection device 30 dynamically monitors the component content of the unadsorbed substances in the flushed liquid; in the process, only the electromagnetic valve on the branch pipe corresponding to the flushing liquid is opened, and other electromagnetic valves are closed. After the flushing is finished, the suction device 10 sucks eluent, the eluent is conveyed to the separation device 20 through the conveying pipeline 40, the specified components adsorbed by the separation device 20 are eluted, the eluted liquid is conveyed to the detection device 30, and the detection device 30 dynamically detects the component content in the eluted liquid; in the process, only the electromagnetic valve on the branch pipe corresponding to the eluent is opened, and other electromagnetic valves are closed. Finally, the suction device 10 sucks the flushing liquid again, the flushing liquid sequentially washes the suction device 10 and the separation device 20 through the conveying pipeline 40, and residual eluent is washed out, so that the conveying pipeline 40, the suction device 10 and the separation device 20 are ensured to be clean and used in subsequent experiments.
The dynamic separation process research and analysis system can dynamically adsorb, separate, elute and dynamically detect components of the predetermined substances in the liquid to be detected, so as to obtain dynamic separation data of the predetermined substances, provide accurate data reference for screening out the adsorption substances with strong adsorption capacity and high adsorption efficiency, and facilitate industrial popularization and application of the adsorption substances with high adsorption capacity and rapid adsorption capacity verified by experimental results.
In order to reduce the amount of liquid to be detected and the amount of eluent, the dynamic separation process research and analysis system further comprises a bubbling device 60, wherein the bubbling device 60 is arranged between the separation device and the detection device, and specifically, an input pipe of the bubbling device 60 is communicated with the third pipeline 43. Specifically, the included angle between the input pipe of the frothing device 60 and the third pipe 43 is an acute angle to the side of the detecting device 30, i.e. the component of the input pipe of the frothing device 60 in the length direction of the third pipe 43 is consistent with the flow direction of the liquid passing through the third pipe 43. The frothing device 60 acts to slow down the liquid flowing through the third pipe 43 during the feeding of the gas; meanwhile, due to the input of gas, the liquid is separated to form a section of liquid separated by the gas, so that the consumption of liquid to be detected and eluent is reduced while the dynamic detection is satisfied.
Example 1
As shown in fig. 2, the dynamic separation process research and analysis system adopting the three-valve structure is used for carrying out the on-line dynamic adsorption separation process research on cadmium. Wherein the suction device adopts a peristaltic pump. The separation device adopts an adsorption column filled with modified anion exchange resin. Wherein the modified anion exchange resin is an adsorption substance and can be replaced. The electromagnetic valve is composed of three two-position two-way electromagnetic valves, and can be a diaphragm valve or a squeeze valve. The detection device is a single-channel detector such as an atomic absorption photometer, and can also be a multi-channel detector such as a plasma spectrometer or a plasma mass spectrometer. Before separation, the three solenoid valves are all in a normally closed state, and the three solenoid valves are respectively numbered as a valve 1, a valve 2 and a valve 3 in sequence. Wherein the valve 1 corresponds to a container for containing flushing liquid, and the flushing liquid adopts purified water; the valve 2 corresponds to a container for containing liquid to be detected; the valve 3 corresponds to a container containing an eluent. During operation, valves 1 to 3 are programmed to open and close. The water, the liquid to be detected and the eluent are respectively input through the valve 1, the valve 2 and the valve 3. The liquid to be detected is a multi-component mixed solution containing cadmium and other base metal elements, and a sample is used for representing the liquid to be detected in the figure. During operation, the peristaltic pump is turned on. Firstly, the valve 1 is opened, so that water is input into the micro adsorption column through the peristaltic pump to clean residual liquid, the micro column outputs the residual liquid to the detector to obtain a dynamic detection signal, and residual components in the residual liquid can be judged according to the strength of the signal. And secondly, the valve 1 is closed, the valve 2 is opened, the liquid to be detected is input into the micro column through the peristaltic pump, the adsorption components are selectively adsorbed by the micro column, and as the adsorption is possibly incomplete, the part which is not adsorbed is input into the detector along with the solution to obtain a dynamic signal, the adsorption efficiency can be judged according to the strength of the signal, and the weaker the signal is, the higher the adsorption efficiency is indicated. And thirdly, closing the valve 2, opening the valve 1, inputting water to the micro adsorption column through the peristaltic pump to flush the unadsorbed components, inputting the components to the detector to obtain a dynamic detection signal, and further judging the unadsorbed proportion, mainly the residual quantity in the resin gaps, according to the strength of the signal. And fourthly, closing the valve 1, opening the valve 3, inputting the eluent into a micro adsorption column through a peristaltic pump, eluting the adsorbed component, inputting the adsorbed component into a detector to obtain a dynamic signal, judging the adsorption quantity according to the strength of the signal, and judging the desorption efficiency according to the shape of the dynamic signal. Fifth, valve 3 was closed and valve 1 was opened, water was fed into the mini-column via peristaltic pump to wash out residual eluent and the column was flushed clean for the next experiment. Finally, according to the second, third and fourth steps, the dynamic signals are relatively strong and weak, and the adsorption efficiency and the elution efficiency can be judged. If a single-channel detector is used, each element needs to be tested step by step, and each set of test conditions needs to be repeated for multiple times to check the adsorption and desorption properties of each element. If a multi-channel detector is used, the adsorption and desorption properties of all elements can be obtained simultaneously, and each set of experimental conditions does not need to be repeatedly checked for each element. In an ideal state, cadmium is required to be completely adsorbed, other elements are required to be adsorbed in zero, at the moment, the detection signals of the cadmium in the second and fourth steps are required to be zero, the detection signals of the other elements in the second step are required to be strongest, the detection signals of the cadmium in the third step are required to be strongest, the detection signals of the other elements are required to be zero, and meanwhile, the detection signals of the cadmium in the third step are required to have no serious tailing.
Example two
As shown in fig. 3, the dynamic separation process research and analysis system adopting the four-valve structure performs the on-line dynamic adsorption separation process research on mercury. Wherein the suction device adopts a peristaltic pump. The separation device adopts an adsorption column filled with strong acid cation exchange resin particles. Wherein, the strong acid cation exchange resin particles are adsorption substances and can be replaced. The electromagnetic valve is composed of four two-position two-way electromagnetic valves, and can be a diaphragm valve or a squeeze valve. The detection device is a single-channel detector such as an atomic absorption photometer, and can also be a multi-channel detector such as a plasma spectrometer or a plasma mass spectrometer. Before separation, the four solenoid valves are all normally closed, and are numbered sequentially as valve 1, valve 2, valve 3 and valve 4. Wherein the valve 1 corresponds to a container for containing flushing liquid, and the flushing liquid adopts purified water; valve 2 and holding to be inspectedThe container corresponding valve 3 of the liquid corresponds to a container for containing the eluting solution potassium bromide, and in the figure, a sample is used for representing the liquid to be detected; the valve 4 corresponds to a container containing the eluent hydrochloric acid. During operation, valves 1 to 4 are programmed to open and close. The input of water, liquid to be detected and eluent is controlled by valves 1, 2, 3 and 4 respectively. The first step, peristaltic pump is opened, valve 1 is opened, water is input to clean peristaltic pump and exchange column; secondly, closing the valve 1, opening the valve 2, inputting mercury-containing liquid to be detected into an ion exchange column, and adsorbing metal cations; third, the valve 2 is closed, the valve 1 is opened, and the ion exchange column is washed by water; fourth, valve 1 is closed and valve 3 is opened, hg is selectively desorbed by 0.1. 0.1M potassium bromide (KBr) solution 2+ The ion, because mercury exists in the form of cation, can be used for acidifying the output liquid of the ion exchange column and adding Hg by introducing the mixed solution of hydrochloric acid and sodium borohydride into a third pipeline between the adsorption column and the detector 2+ Examples reduction to Hg atoms for detection; of course, for simple structure, the exchange column filled with the mercapto resin can be directly used for adsorption without introducing the mixed solution of hydrochloric acid and sodium borohydride into the third pipeline, but the mercapto resin is expensive. Fifthly, closing the valve 3, opening the valve 4, inputting 1M hydrochloric acid (HCl) to elute all adsorbed metal cations and conveying the eluted metal cations to a detector for detection; sixth, valve 4 is closed, valve 1 is opened, and water is fed to clean the ion exchange column and the linked tubing for the next cycle. According to the relative intensity of detection signals of various elements in the second, third, fourth and fifth steps, the adsorption and desorption efficiency can be judged, so that the mercury separation efficiency is judged. For example, if the detection signals of the various elements in the second step are weak, the surface adsorption efficiency is high; if the mercury signal is strong and the other element signals are weak in the third step, the surface separation efficiency is high. Elemental detection may be performed by a single channel detector, such as an atomic absorption photometer, but individual elements may be tested serially, or simultaneously by a multi-channel detector, such as a plasma spectrometer or a plasma mass spectrometer.
Example III
As shown in fig. 4, a dynamic separation process study and a dynamic separation process using a six-valve structureAnalysis System for arsenic (A) S ) And (5) researching an online dynamic adsorption separation process. Wherein the suction device adopts a peristaltic pump. The separation device adopts an adsorption column filled with polystyrene anion exchange resin particles. Wherein, the polystyrene anion exchange resin particles are adsorption substances and can be replaced. The electromagnetic valve adopts four single-channel electromagnetic valves and two double-channel extrusion valves; the valves are numbered in order as valve 1, valve 2, valve 3, valve 4, valve 5 and valve 6, respectively. Wherein, valve 1, valve 2, valve 4 and valve 5 are two-position two-way diaphragm valve or single-channel extrusion valve, valve 3 and valve 5 are two-way extrusion valve, two channels of valve 3 are normally closed, one channel of valve 5 is normally open, the other channel is normally closed, and valve 1 and valve 4 are normally open. During operation, valves 1 to 6 are programmed to open and close. The valve 1 corresponds to flushing liquid, and the flushing liquid adopts purified water; the valve 2 corresponds to the liquid to be detected, and the liquid to be detected is represented by a sample in the figure; valve 3 corresponds to the eluent dilute acid and the reducing agent sodium borohydride, valve 4 corresponds to water, valve 5 corresponds to the concentrated acid, and valve 6 corresponds to potassium iodide (KI) and water. The detection device is a single-channel detector such as an atomic absorption photometer, and can also be a multi-channel detector such as a plasma spectrometer or a plasma mass spectrometer. When the peristaltic pump is used, the peristaltic pump is started, the valve 1 is started first, the normally open ends of the valve 4 and the valve 6 are in an open state, so that water is input into the micro adsorption column and the pipeline system through the peristaltic pump to clean residual liquid, and the micro column outputs the residual liquid to the detector. In the second step, valve 1 is closed and valve 2 is opened, the liquid to be detected is fed into the mini column by peristaltic pump, the component to be adsorbed (As 5+ ) The adsorption by the micro column is possible to be incomplete, and the part which is not adsorbed is input into the detector along with the solution, so that the detector can dynamically detect. Third, valve 2 is closed and valve 1 is opened, water is fed to the micro adsorption column via peristaltic pump to flush out non-adsorbed components and fed to the detector. Fourth, valve 1 is closed, valve 3 is opened, eluent (dilute acid) is fed into the micro adsorption column through peristaltic pump, and As to be adsorbed 5+ Eluting while the reducing agent is fed to the third conduit via valve 3 and peristaltic pump and is combined with As 5+ Ion reaction to generate As atoms, dynamic detection by detector, and judging adsorption quantity and arsenic concentration according to signal strengthThe elution efficiency can be judged. Fifth, valve 3 is closed and valve 1 is opened, concentrated acid is fed into the micro-adsorption column via peristaltic pump to remove residue A S 5+ The ions elute clean to regenerate the adsorption column. And sixth, the valve 5 is closed, the valve 1 is opened, and water is fed into the micro adsorption column and the reaction pipeline through the constant ends of the valve 1, the valve 4 and the valve 6 and the peristaltic pump to be cleaned for the next experiment. In the above process, argon is continuously blown into the third pipeline through the bubbling device, so that the liquid to be detected is isolated by gas, and the amount of the liquid to be detected is reduced, namely, the separation and analysis process can be completed by reducing the amount of the liquid to be detected and the eluent.
In the above-described embodiments, the residual components in the residual liquid in the transfer line 40, the suction device 10, and the separation device 20 can be reduced by the cleaning. However, since the first pipeline 41 adopts a plurality of branch pipes, the branch pipes corresponding to water can be washed cleanly, and other branch pipes are not washed, so that the accuracy of the next experimental result is affected; if the tube is directly replaced, the tube is replaced in each experiment, so that the experiment cost is greatly increased.
In order to solve the problems in the above technical solutions, embodiments of the present application continue to propose optimization improvements to the above technical solutions. In comparison with the above-described solution, the main difference is that the number of first pipes 41 of the conveying pipe 40 is one. In order to match with the dynamic separation process research and analysis system, the system also comprises a storage device for storing the liquid to be detected, water and reagent solution. The storage device includes a storage table 70 and a drive motor. The storage table 70 has a degree of freedom of rotation about a fixed axis, and a plurality of storage grooves 71 for storing containers are provided thereon in a direction about the axis of rotation. The driving motor is connected with the bottom of the circular object placing table 70 and is used for driving the circular object placing table 70 to horizontally rotate. Before use, the liquid to be tested, water and reagent solution are placed in the storage tank 71 of the storage table 70 in a set order. In use, the first tube 41 is inserted into the corresponding container containing the drug by rotating the table 70. The first conduit 41 should be bendable so as to extend into the container in the storage tank 71. Meanwhile, in the technical scheme, only one electromagnetic valve is needed, so that the experimental cost investment can be reduced.
Specifically, the first pipe 41 includes a first hard pipe 411, a second hard pipe 412, and a first hose 413. Wherein both ends of the first hose 413 are connected to the first hard tube 411 and the second hard tube 412, respectively. Meanwhile, the first pipeline 41 is further provided with a driving device 80, and the driving device 80 can drive the first pipeline 41 to stretch and bend. The drive 80 includes a housing block 81, a cylinder 82, a motor 83, and a gear set 84. Wherein the number of the sleeve blocks 81 is two. And, the middle parts of the two sleeve blocks 81 are provided with through holes. The two sleeve blocks 81 are respectively arranged on the first hard tube 411 and the second hard tube 412. The two ends of the cylinder 82 are rotatably connected with the sides of the two sleeve blocks 81. The distance between the first hard pipe 411 and the second hard pipe 412 can be adjusted by the expansion and contraction of the cylinder 82, thereby realizing the extension and shortening of the first pipe 41. The motor 83 is provided on one of the jacket blocks 81. A gear set 84 is provided between the output shaft of the motor 83 and the cylinder 82. Specifically, the gear set 84 includes a first gear and a second gear engaged with the first gear, where the first gear is sleeved on the output shaft of the motor 83, and the second gear is fixedly connected to one end of the cylinder 82. The motor 83 drives the second gear to rotate through the first gear, so that the rotation of the air cylinder 82 is realized, and the first hard pipe 411 rotates relative to the second hard pipe 412 through the rotation of the air cylinder 82, so that the bending of the first pipeline 41 is realized. The first pipe 41 is bent, so that the first pipe 41 can be conveniently inserted into the container in the storage groove 71.
Before the application process, the containers containing water, liquid to be detected and eluent are placed in a certain sequence in the storage tank 71 of the storage table 70. When a sample needs to be separated and analyzed, the driving motor 83 drives the object placing table 70 to rotate, so that the container for containing water corresponds to the first pipeline 41, the driving device 80 drives the first pipeline 41 to rotate, the first pipeline 41 stretches into the container below the water surface, the suction device 10 absorbs water, the water sequentially passes through the suction device 10 and the separation device 20 through the conveying pipeline 40, and the detection device 30 detects residual components in the washed liquid. After the flushing is finished, the driving device 80 drives the first pipeline 41 to straighten so as to withdraw from the container containing water, then the driving motor 83 drives the object placing table 70 to rotate by a set angle, so that the container containing the liquid to be detected corresponds to the first pipeline 41, the driving motor 83 drives the first pipeline 41 to bend, the liquid to be detected is stretched into the container containing the liquid to be detected to suck the liquid to be detected, the liquid to be detected sequentially passes through the suction device 10 and the separation device 20 through the conveying pipeline 40, the separation device 20 adsorbs specified components in the liquid to be detected, the adsorbed liquid is conveyed to the detection device 30, and the detection device 30 dynamically detects residual components in the adsorbed liquid. The cycle is followed by the elution and detection of the aspirated eluent, and the washing of the transfer line 40, the aspiration device 10 and the separation device 20 by the aspiration of water for subsequent use in experiments. In the improved technical scheme, all the conveying pipelines 40, the suction devices 10 and the separation devices 20 can be cleaned, and the accuracy of the results of subsequent experiments can be improved; and the first pipe 41 does not need to be replaced frequently, so that the rise of experiment cost is avoided.
Although embodiments of the present invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made therein without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (9)
1. A method of analysis of a dynamic separation process research and analysis system, the dynamic separation process research and analysis system comprising:
suction means for sucking the liquid;
a separation device filled with a replaceable adsorption material for separating a predetermined material in the liquid output from the suction device;
the detection device is used for detecting the content of each component of the output liquid of the separation device;
the liquid storage device is at least three groups of liquid storage devices respectively used for containing cleaning liquid, eluent and liquid to be detected, and in the working state, the outlet ends of the liquid storage devices are respectively communicated with the inlet ends of the suction devices, and a first passage used for circulating the cleaning liquid to clean the system, a second passage used for circulating the liquid to be detected and adsorbing and detecting the predetermined substances therein, and a third passage used for circulating the eluent and eluting and detecting the adsorbed predetermined substances are respectively formed;
the analysis method comprises the following steps:
step 1: the suction device sucks the cleaning liquid, the cleaning liquid sequentially passes through the suction device and the separation device and is washed, and the detection device detects residual components in the washed liquid;
step 2: the suction device sucks liquid to be detected, the liquid to be detected sequentially passes through the suction device and the separation device, the separation device adsorbs preset substances in the liquid to be detected, the adsorbed liquid is conveyed to the detection device, the detection device dynamically detects the adsorbed liquid, and the adsorption efficiency of the preset substances is judged according to the dynamic detection signal;
step 3: the suction device sucks the cleaning liquid, the cleaning liquid sequentially passes through the suction device and the separation device and is washed, the washed liquid is conveyed to the detection device, and the detection device dynamically detects the content of unadsorbed components in the washed liquid;
step 4: the suction device sucks the eluent and conveys the eluent to the separation device, the eluent elutes the predetermined substances adsorbed in the separation device, the eluted liquid is conveyed to the detection device, the detection device dynamically detects the eluted liquid, and the eluting efficiency of the predetermined substances is judged according to the dynamic detection signal;
step 5: the suction device sucks the cleaning liquid, and the cleaning liquid sequentially passes through the suction device and the separation device to wash out residual eluent.
2. The method of claim 1, wherein the dynamic separation process research and analysis system further comprises a first pipeline connecting the liquid storage device and the pumping device, and a valve body assembly for controlling the on-off of the first pipeline is arranged on the first pipeline.
3. The method of claim 2, wherein the first conduit comprises a plurality of branches connected in parallel and a manifold connected to the branches; the branch pipes are correspondingly communicated with the liquid storage device; the main pipe is communicated with the inlet end of the suction device; the valve body assembly comprises a plurality of electromagnetic valves which are arranged on the branch pipes in a one-to-one correspondence manner.
4. The method of claim 2, wherein dynamically separating and analyzing the reservoir further comprises:
the object placing table is provided with a degree of freedom for rotating around a fixed axis, a plurality of object placing grooves for placing containers are formed in the top surface of the object placing table around the direction of the rotating axis, and the containers are used for containing cleaning liquid, eluent and liquid to be detected;
the driving motor is connected with the bottom of the circular object placing table and is used for driving the circular object placing table to horizontally rotate;
the number of the first pipelines is one, and the first pipelines can be bent and extend into the container in the storage groove.
5. The method according to claim 4, wherein the first pipeline comprises a first hard pipe, a second hard pipe, a first hose with two ends respectively connected with the first hard pipe and the second hard pipe, and a driving device arranged on the first pipeline and used for driving the first pipeline to stretch and bend.
6. The method of claim 5, wherein the driving means comprises:
the middle part of the sleeve block is provided with two through holes, and the sleeve block is sleeved on the first hard tube and the second hard tube respectively;
the two ends of the air cylinder are respectively connected with the side edges of the two sleeve blocks in a rotating way;
the motor is arranged on one of the sleeve blocks;
the gear set is connected with the motor output shaft and the air cylinder in a transmission way.
7. The method of claim 3, wherein the solenoid valve is a diaphragm solenoid valve and/or a hose squeeze valve.
8. The method of claim 1, wherein the aspiration device employs a peristaltic pump.
9. The method of claim 1, wherein the dynamic separation process research and analysis system further comprises a bubbling device disposed between the separation device and the detection device.
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