CN114849281A - Liquid chromatogram pulse type sample injection control device and control method for nuclide separation - Google Patents
Liquid chromatogram pulse type sample injection control device and control method for nuclide separation Download PDFInfo
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D15/00—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
- B01D15/08—Selective adsorption, e.g. chromatography
- B01D15/10—Selective adsorption, e.g. chromatography characterised by constructional or operational features
- B01D15/14—Selective adsorption, e.g. chromatography characterised by constructional or operational features relating to the introduction of the feed to the apparatus
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D15/00—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
- B01D15/08—Selective adsorption, e.g. chromatography
- B01D15/10—Selective adsorption, e.g. chromatography characterised by constructional or operational features
- B01D15/16—Selective adsorption, e.g. chromatography characterised by constructional or operational features relating to the conditioning of the fluid carrier
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/008—Control or steering systems not provided for elsewhere in subclass C02F
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/006—Radioactive compounds
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- C—CHEMISTRY; METALLURGY
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- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/08—Seawater, e.g. for desalination
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2209/00—Controlling or monitoring parameters in water treatment
- C02F2209/42—Liquid level
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E30/00—Energy generation of nuclear origin
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Abstract
The invention discloses a liquid chromatogram pulse type sample injection control device and a control method for nuclide separation, which comprises a box body; the input piece is arranged on one outer side wall of the box body, the output end of the input piece is communicated with the box body, the input piece is provided with an air inlet end and a liquid inlet end, and the air inlet end and the liquid inlet end work in a linkage mode; the output piece is arranged on the other outer side wall of the box body, which is far away from the input piece, the input end of the output piece is communicated with the box body, the output piece is provided with a first liquid outlet end and a second liquid outlet end, and the first liquid outlet end and the second liquid outlet end work in a linkage manner; the control piece is arranged outside the box body and used for controlling the opening and closing of the air inlet end, the liquid inlet end, the first liquid outlet end and the second liquid outlet end. The invention can solve the problem that the separation is difficult to realize due to continuous sample introduction in the liquid chromatography separation. When the sample is injected in a pulse mode, a chromatographic column does not need to be washed, and particularly, when sample liquid comes out of the chromatographic column, nuclide separation can be carried out according to the optimal separation time point.
Description
Technical Field
The invention relates to the technical field of nuclide separation devices, in particular to a liquid chromatogram pulse type sample injection control device and a control method for nuclide separation.
Background
High Performance Liquid Chromatography (HPLC) is developed rapidly by introducing gas chromatography theory in the late 60's of the 20 th century on the basis of classical liquid chromatography. The difference from classical liquid chromatography is that the filler particles are small and uniform. Since smaller packed particles have high column efficiency but cause high resistance, high pressure transport of the mobile phase is required, and is also known as high pressure liquid chromatography. When the high performance liquid chromatography is used, a solution to be detected is injected into a chromatographic column and moves in a fixed phase through pressure, different substances sequentially leave the chromatographic column due to different types of detected substances and different interaction between the substances and the fixed phase, different peak signals are obtained through a detector, and finally the substances contained in the to-be-detected substances are judged through analyzing and comparing the signals. High performance liquid chromatography is widely used in chemical and biochemical analysis as an important analytical method. The high performance liquid chromatography has no essential difference from the classical liquid chromatography in principle, and is characterized by adopting a high-pressure infusion pump, a high-sensitivity detector and a high-efficiency particle stationary phase, and being suitable for analyzing organic compounds with high boiling points, difficult volatilization, large molecular weight and different polarities. High performance liquid chromatography is used in a wide variety of applications, almost throughout the field of quantitative and qualitative analysis.
High performance liquid chromatography requires only that the sample be made into a solution, is not limited by the volatility of the sample, has a wide selection range of mobile phases, and a wide variety of stationary phases, and thus can separate thermally unstable and non-volatile, dissociated and non-dissociated, and various molecular weight ranges of substances. By matching with a sample pretreatment technology, the high resolution and the high sensitivity achieved by the high performance liquid chromatography can separate and simultaneously measure substances with very similar properties, and can separate trace components in a complex mixture. And with the development of the stationary phase, the separation of the biochemical substances can be completed under the condition of fully maintaining the activity of the biochemical substances. Since the high performance liquid chromatography has the advantages of high resolution, high sensitivity, high speed, repeated utilization of chromatographic columns, easy collection of effluent components and the like, the method is widely applied to various fields of biochemistry, food analysis, medical research, environmental analysis, inorganic analysis and the like, and becomes the most promising method for solving the problem of biochemical analysis.
However, the traditional chromatography still has some problems, firstly, in separation, because the traditional chromatography belongs to continuous sample injection, the substantive and meaningful separation of a sample is difficult to realize, secondly, the separation time is difficult to determine, meanwhile, the traditional chromatograph is mainly applied to the analysis fields of analytical chemistry, organic chemistry, biochemistry and the like, the research of the chromatography for the separation fields of nuclide separation, uranium extraction from seawater and the like is rare, and finally, the quality of the chromatographic separation performance in the past depends on the type and the property of a stationary phase to a great extent, but the difference of the sample injection mode, the performance of each component and the mechanism of the interaction between the sample injection mode, the performance of each component and the stationary phase are ignored.
Disclosure of Invention
The invention aims to provide a liquid chromatogram pulse type sample injection control device and a control method for nuclide separation, which are used for solving the problems in the prior art and solving the problems that continuous sample injection is difficult to realize separation in liquid chromatogram separation. When the sample is injected in a pulse mode, a chromatographic column does not need to be washed, and particularly, when sample liquid comes out of the chromatographic column, nuclide separation can be carried out according to the optimal separation time point.
In order to achieve the purpose, the invention provides the following scheme: the invention provides a liquid chromatogram pulse type sample injection control device for nuclide separation, which comprises,
a box body;
the input piece is arranged on one outer side wall of the box body, the output end of the input piece is communicated with the box body, the input piece is provided with an air inlet end and a liquid inlet end, and the air inlet end and the liquid inlet end work in a linkage mode;
the output piece is arranged on the other outer side wall of the box body, which is far away from the input piece, the input end of the output piece is communicated with the box body, the output piece is provided with a first liquid outlet end and a second liquid outlet end, and the first liquid outlet end and the second liquid outlet end work in a linkage manner;
the control element is arranged outside the box body and used for controlling the opening and closing of the air inlet end, the liquid inlet end, the first liquid outlet end and the second liquid outlet end;
the monitoring piece is arranged in the box body and used for monitoring the height of the solution in the box body, and the monitoring piece is electrically connected with the control piece.
Preferably, the control includes a control panel, the rigid coupling has first relay on the input piece, the control panel with first relay electric connection, first relay control the inlet end with during the output intercommunication of input piece, the feed liquor end with the output of input piece is closed, first relay control the inlet end with during the output of input piece is closed, the feed liquor end with the output intercommunication of input piece.
Preferably, a second relay is fixedly connected to the output piece, the control panel is electrically connected to the second relay, the second relay controls the first liquid outlet end to be communicated with the input end of the output piece, the second liquid outlet end is closed to the input end of the output piece, and the second relay controls the first liquid outlet end to be communicated with the input end of the output piece when the first liquid outlet end is closed to the input end of the output piece.
Preferably, the input part comprises an input three-way valve fixedly connected with the outer side wall of the box body, the liquid outlet end of the input three-way valve is communicated with the inside of the box body, the air inlet end of the input three-way valve is communicated with the outside air through an air inlet pipe, and the liquid inlet end of the input three-way valve is communicated with the primary sample pool through a liquid inlet pipe.
Preferably, the output piece include with the output three-way valve of box lateral wall rigid coupling, output three-way valve feed liquor end with intercommunication in the box, the first play liquid end of output three-way valve has primary sample backward flow pond through first drain pipe intercommunication, the second play liquid end of output three-way valve has secondary sample backward flow pond through second drain pipe intercommunication.
Preferably, the outer wall rigid coupling of box has the peristaltic pump, the peristaltic pump is used for the drive intake pipe conveying gas, the peristaltic pump is used for the drive the feed liquor pipe first drain pipe the second drain pipe conveying solution.
Preferably, the monitoring part comprises a liquid level sensor fixedly connected with the inner wall of the box body, and the liquid level sensor is electrically connected with the control panel.
Preferably, the outer wall of the box body is fixedly connected with a display screen, and the display screen is electrically connected with the control panel.
The control method of the liquid chromatogram pulse type sampling control device for nuclide separation comprises the following operation steps:
s1, determining an initial position: starting the control element and the monitoring element, communicating the air inlet end of the input element with the box body, and communicating the first liquid outlet end of the output element with the box body;
s2, setting the operation time: setting the communication time of the air inlet end of the input piece and the box body to be T, setting the communication time of the liquid inlet end of the input piece and the box body to be T2, and setting the communication time of the first liquid outlet end of the output piece and the box body to be T3;
s3, tank liquid inlet: the control piece works, after the air inlet end of the input piece is communicated with the box body for T time, the liquid inlet end of the input piece is communicated with the box body, and after the air inlet end of the input piece is communicated for T2 time, the input piece stops working;
s4, draining liquid by a box body: the monitoring part monitors that the solution in the box body rises to a certain height and then feeds back the solution to the control part, and after the control part controls the first liquid outlet end of the output part to be communicated with the box body for T3, the second liquid outlet end of the output part is communicated with the box body;
s5, resetting the device: the monitoring part monitors that the solution in the box body descends to a certain height and then feeds back the solution to the control part, the control part controls the air inlet end of the input part to be communicated with the box body, and the first liquid outlet end of the output part is communicated with the box body.
Preferably, in step S2, time T3 is less than time T2.
The invention discloses the following technical effects:
1. compared with a traditional liquid chromatograph, the device has the advantages of a liquid chromatogram pulse type sample injection control device, solves the problems of the traditional liquid chromatograph, adopts a part of sample injection form through the matching of an input part and an output part, solves the problem that the separation is difficult to realize by continuous sample injection in the separation, does not need leaching, and can determine the optimal separation time point.
2. The traditional chromatograph is mainly applied to the fields of analytical chemistry, organic chemistry, biochemistry and the like, and the pulse type sample injection device and the control method thereof are mainly applied to the aspects of nuclide separation and concentration.
3. The liquid chromatogram pulse type sampling control device can be used for extracting uranium from seawater in a laboratory. On the basis of a pulse nuclide separation system, effective separation and extraction of uranium elements in a seawater sample are realized under the optimal experimental conditions and experimental stages, and a product is fixed in a yellow cake form. Because the content of uranium in seawater is extremely low, the currently adopted uranium adsorption extraction method has the scientific problems of complex reaction mechanism, limited adsorption capacity, great influence by external environment and the like, and has the difficult problems of high cost, low efficiency, difficulty in realizing batch production and the like. The method is expected to solve the series of scientific and economic problems.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings needed to be used in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings without inventive exercise.
FIG. 1 is a schematic structural diagram of a control device;
FIG. 2 is a perspective view of the input member;
FIG. 3 is a perspective view of the output member;
FIG. 4 is a front view of the control panel;
FIG. 5 is a schematic view of the connection of a control line to a fluid line;
FIG. 6 is a graph of example 1;
FIG. 7 is a graph of example 2;
the system comprises a box body 1, a control panel 2, a first relay 3, a second relay 4, an input three-way valve 5, an air inlet pipe 6, a liquid inlet pipe 7, a primary sample pool 8, an output three-way valve 9, a first liquid outlet pipe 10, a primary sample return pool 11, a second liquid outlet pipe 12, a secondary sample return pool 13, a peristaltic pump 14, a liquid level sensor 15, a display screen 16, a MCU (micro control unit) main control panel 17, a power switch 18, a peristaltic pump switch 19, a peristaltic pump driving circuit 20, a control line 21 and a liquid pipeline 22.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
In order to make the aforementioned objects, features and advantages of the present invention comprehensible, embodiments accompanied with figures are described in further detail below.
Referring to fig. 1-7, the present invention provides a liquid chromatography pulse type sample injection control device for nuclide separation, which comprises a box body 1; the input piece is arranged on one outer side wall of the box body 1, the output end of the input piece is communicated with the box body 1, the input piece is provided with an air inlet end and a liquid inlet end, and the air inlet end and the liquid inlet end work in a linkage mode; the output piece is arranged on the other outer side wall of the box body 1 far away from the input piece, the input end of the output piece is communicated with the box body 1, the output piece is provided with a first liquid outlet end and a second liquid outlet end, and the first liquid outlet end and the second liquid outlet end work in a linkage mode; the control piece is arranged outside the box body 1 and is used for controlling the opening and closing of the air inlet end, the liquid inlet end, the first liquid outlet end and the second liquid outlet end; the monitoring piece is arranged in the box body 1 and used for monitoring the height of the solution in the box body 1, and the monitoring piece is electrically connected with the control piece.
The control piece is used for controlling the work of the input piece and the output piece, the liquid inlet end of the input piece can be used for introducing gas into the box body 1 and can also be used for introducing solution into the box body 1, the first liquid outlet end and the second liquid outlet end of the output piece can discharge the solution in the box body 1, the liquid level height in the box body 1 is monitored through the monitoring piece, and therefore the opening and closing of the gas inlet end, the liquid inlet end, the first liquid outlet end and the second liquid outlet end are controlled.
Further optimization scheme, control piece include a control panel 2, and the rigid coupling has first relay 3 on the input, control panel 2 and 3 electric connection of first relay, and when 3 control inlet ends of first relay communicate with the output of input, the feed liquor end is closed with the output of input, and when 3 control inlet ends of first relay were closed with the output of input, the feed liquor end communicates with the output of input. Under the effect of first relay 3 for the output of input member only can with inlet end or feed liquor end intercommunication, through the switching of inlet end and feed liquor end, thereby realize to the interior input gas of box 1 or input solution.
According to the further optimization scheme, the second relay 4 is fixedly connected to the output piece, the control panel 2 is electrically connected with the second relay 4, when the second relay 4 controls the first liquid outlet end to be communicated with the input end of the output piece, the second liquid outlet end is closed to the input end of the output piece, and when the second relay 4 controls the first liquid outlet end to be closed to the input end of the output piece, the second liquid outlet end is communicated with the input end of the output piece. The input piece inputs solution into the box 1, so that the liquid level in the box 1 rises, the monitoring liquid level height of the monitoring piece reaches a preset value, the monitoring liquid level height is fed back to the output piece, the first liquid outlet end of the output piece discharges the solution in the box 1, after a certain time, the liquid level in the box 1 falls to a certain position, the monitoring piece feeds back to the output piece, and the second liquid outlet end of the output piece discharges the residual solution in the box 1.
As shown in fig. 4-5, the control board 2 is a 4 × 4 keyboard, a start/stop key and a time adjusting member are provided on the keyboard, and are used for controlling the first relay 3 and the second relay 4, the control board 2 is electrically connected with an MCU main control board 17, the first relay 3 and the second relay 4 are controlled by the MCU main control board 17 to operate, so as to control the input member and the output member at different times, so that the input member firstly introduces gas into the box 1 within a set time, and then introduces solution into the box 1, and the output member discharges the solution in the box 1 from the first liquid outlet end within the set time, and discharges the solution in the box 1 from the second liquid outlet end at another time. A power switch 18 is fixedly connected to the outer wall of the box body 1 to electrify each device, so that each electronic device can work normally.
Further optimize the scheme, the input piece includes with the input three-way valve 5 of 1 lateral wall rigid coupling of box, the play liquid end and the box of input three-way valve 5 in the intercommunication, the inlet end of input three-way valve 5 passes through intake pipe 6 and outside air intercommunication, the feed liquor end of input three-way valve 5 has elementary sample cell 8 through feed liquor pipe 7 intercommunication. The input three-way valve 5 is provided with a liquid outlet end, a gas inlet end and a liquid inlet end, wherein the liquid outlet end can also pass gas, the gas inlet end is firstly communicated with the liquid outlet end under the action of the first relay 3, the gas is input into the box body 1, the liquid inlet end is communicated with the liquid outlet end after a certain time, and the solution in the primary sample pool 8 is input into the box body 1 through the liquid inlet pipe 7.
Further optimize the scheme, output spare includes the output three-way valve 9 with the lateral wall rigid coupling of box 1, and output three-way valve 9 feed liquor end communicates in with the box 1, and the first play liquid end of output three-way valve 9 has primary sample backward flow pond 11 through first drain pipe 10 intercommunication, and the second play liquid end of output three-way valve 9 has secondary sample backward flow pond 13 through second drain pipe 12 intercommunication. The output three-way valve 9 has an input, a first output, a second output, after the liquid level in the box 1 reached a definite value, the input communicates with first output, the solution in the box 1 is exported to primary sample backward flow pond 11 in by first drain pipe 10, treat after a certain time, liquid level descends in the box 1, the input communicates with the second output, remaining solution in the box 1 is exported to secondary sample backward flow pond 13 in by second drain pipe 12 in, input spare and output spare reset afterwards, continue next separation process.
According to the further optimization scheme, the outer wall of the box body 1 is fixedly connected with a peristaltic pump 14, the peristaltic pump 14 is used for driving the air inlet pipe 6 to convey air, and the peristaltic pump 14 is used for driving the liquid inlet pipe 7, the first liquid outlet pipe 10 and the second liquid outlet pipe 12 to convey solution. The peristaltic pump 14 is used for providing power, meanwhile, the peristaltic pump 14 is controlled by the MCU main control board 17, and the MCU main control board 17 drives the peristaltic pump 14 to work through the peristaltic pump driving circuit 20, so that the power transmission object and the power transmission time of the peristaltic pump are controlled, and the device works normally. A peristaltic pump switch 19 is fixedly connected to the outer wall of the box body 1 to start or stop the peristaltic pump 14.
Further optimize the scheme, the monitoring part includes the level sensor 15 with 1 inner wall rigid coupling of box, level sensor 15 and control panel 2 electric connection. The liquid level sensor 15 is used for monitoring the liquid level in the box body 1 so as to feed back to the output piece to enable the output piece to work.
In one embodiment of the present invention, the level sensor 15 is preferably, but not limited to, a capacitive line level sensor.
Further optimize the scheme, the outer wall of the box body 1 is fixedly connected with a display screen 16, and the display screen 16 is electrically connected with the control panel 2. The display screen 16 should be electrically connected with the control board 2 and the MCU main control board so that the adjustment time of the control board 2 can be displayed on the display screen 16 for the experimenter to observe.
The control method of the liquid chromatogram pulse type sampling control device for nuclide separation comprises the following operation steps:
s1, determining an initial position: and starting the control piece and the monitoring piece, communicating the air inlet end of the input piece with the box body 1, and communicating the first liquid outlet end of the output piece with the box body 1. The system is powered on, the air inlet pipe 6 of the input three-way valve 5 is communicated with the output end of the input three-way valve 5, and the input end of the output three-way valve 9 is communicated with the first liquid outlet pipe 10.
S2, setting the operation time: the communication time of the air inlet end of the input element and the box body 1 is set to be T1, the communication time of the liquid inlet end of the input element and the box body 1 is set to be T2, and the communication time of the first liquid outlet end of the output element and the box body 1 is set to be T3. The parameters are adjusted by the control board 2, the time for introducing gas into the box body 1 is T1, for example, the time for T1 is 60 s-70 s (the time can be adjusted according to actual requirements), after the gas introduction is finished, the time for introducing solution into the box body 1 is T2, for example, the time for T2 is 200s (the time can be adjusted according to actual requirements), then the gas is introduced into the box body 1, and the above operations are circulated, so that sampling pulses can be generated. And the display screen 16 displays the various parameters currently set by the system.
S3, feeding liquid into the box body 1: and the control element works, after the air inlet end of the input element is communicated with the box body 1 for T1, the liquid inlet end of the input element is communicated with the box body 1, and after the communication time is T2, the input element stops working. Controlling the sample injection speed according to the performance of the chromatographic column and the separation effect on different nuclides to achieve the balance with the control of the front-end sample injection stage; the chromatographic column can be used for separating different nuclides by connecting a sample separated by the chromatographic column with ICP-MS for analysis.
S4, draining liquid by the box body 1: the monitoring part monitors that the solution in the box body 1 rises to the height of the liquid level sensor 15 and then feeds back the solution to the control part, and after the control part controls the first liquid outlet end of the output part to be communicated with the box body 1 for T3, the second liquid outlet end of the output part is communicated with the box body 1. The combined sample liquid passes through the chromatographic column and then separates and collects each nuclide by controlling the flow direction of the output three-way valve 9. The phase consists of a second relay 4, a peristaltic pump 14, an output three-way valve 9, a liquid level sensor 15, necessary management and lines, is arranged at the outlet of a chromatographic column solution, and automatically controls the trend of the solution by setting the shunting time. The main actions are as follows:
1. the arrival/completion of the solution in the tank 1 is automatically recognized by the level sensor 15.
2. After the solution is identified to arrive, timing is started, the solution flows out from the first liquid outlet pipe 10 of the output three-way valve 9 and enters the primary sample reflux pool 11, and after 200s (time is adjustable), the first liquid outlet pipe 10 is closed, the second liquid outlet pipe 12 is opened, and the solution flows out from the second liquid outlet pipe 12 and enters the secondary sample reflux pool 13.
3. After the solution in the pulse section flows out, the state of the solution flowing out is automatically identified, the second liquid outlet pipe 12 is closed, the first liquid outlet pipe 10 is opened, and subsequent air and solution flow out from the first liquid outlet pipe 10.
4. The above operations 2 and 3 can be performed cyclically.
S5, resetting the device: the monitoring part monitors that the solution in the box body 1 descends to a certain height and then feeds back the solution to the control part, the control part controls the air inlet end of the input part to be communicated with the interior of the box body 1, and the first liquid outlet end of the output part is communicated with the interior of the box body 1. After the above-mentioned process is completed, the input element and output element are reset so as to make nuclide separation of next batch.
Further optimization, in step S2, time T3 is less than time T2. The time T3 for removing the solution from the first outlet pipe 10 to the tank 1 should be shorter than the time for feeding the solution from the inlet pipe 7 to the tank 1 to prevent the first outlet pipe 10 from doing no work when the water is drained.
Example 1
As shown in FIG. 6, the variation of nuclides in the chromatographic column within the pulse time is judged through the pulse sample injection test, so as to primarily analyze the positions of the separation time points of different nuclides, namely, the time of T3 is determined. Firstly, 5mg/L of uranium standard solution, a buffer solution with the pH value of 2.7 and 1g/L of azoarsine III are prepared. The experiment used a 5m long column. According to the device operation method, equipment is debugged. The rotating speed of the sample feeding peristaltic pump 14 is 30r/min, the pulse time T1 is set to be 60S, the sample feeding time T2 is set to be 100S, and the sample feeding amount is 10 mL. The T3 time is not set. According to the set parameters, the operation is carried out, namely, a solution pipeline is connected into the primary sample pool 8, the T1 pulse time is timed, the chromatographic column enters gas, the gas inlet pipe 6 of the input three-way valve 5 is closed when the T1 is finished, the T2 is timed, the liquid inlet pipe 7 of the input three-way valve 5 is opened, and the sample enters the chromatographic column, so that the cycle operation is carried out. And (4) mixing the sample liquid with the color developing agent after the sample liquid comes out of the chromatographic column, entering an online spectrophotometer, and recording data change. The device was operated for the four pulse case with the first pulse data being discarded in each experiment. The absorbance of the graph shows the change of the concentration of the uranium solution at different times after the uranium solution is separated by a chromatographic column. And (3) performing pulse action for three times, wherein the chromatographic column blocks and separates uranium ions just after the solution enters the chromatographic column, and the concentration of the uranium solution in the chromatographic column is continuously increased and the absorbance is also continuously increased along with the increase of the sample volume. When the concentration reaches the highest point, the high-concentration sample liquid leaves the chromatographic column, and the T2 sample introduction time is ended, and T1 is operated to carry out air pulse. The pressure in the chromatographic column is reduced, so that uranium ions are retained in the chromatographic column, and the absorbance is reduced. When the pulse sample liquid in the section is quickly removed, the time T1 is over, the time T2 is running, the pressure in the chromatographic column is increased, the uranium ions move in an accelerated manner, the concentration is increased, and the absorbance is increased.
Example 2
As shown in FIG. 7, a pulsed sample injection device is used for separating and testing the uranium, europium and sodium ion mixed solution, and a 5mg/L uranium standard solution, a 5mg/L europium solution and 1mol/L sodium ion are prepared in an experiment. The peristaltic pump 14 advances kind rotational speed and is 20r/min, advances kind solution and is 25mL, 12mL are respectively got to europium and uranium solution, and 12mL of sodium ion solution are mixed, set up separator's time parameter, and this experiment is a pulse to solution ration advances kind, consequently need not set up T1 and T2 time, only needs to set up T3 separation time point. According to the previous experiment verification, the first 7mL of solution after the chromatographic column is discharged basically has no uranium ions, so that every 3mL of solution from the 8 th mL is taken as a separation point, the separation liquid is collected and the concentration conditions of the three ions are determined, the separation conditions of uranium and europium correspond to each pulse sampling separation in the embodiment 1, and the ion concentration fluctuation is similar. According to the uranium and sodium ion separation in example 2, the T3 separation point time of the uranium and sodium ions can be determined to be the last 3mL of sample liquid in the chromatographic column. The operability and feasibility of the liquid chromatogram pulse type sampling device are verified, and the scientificity of the pulse type sampling method is verified at the same time.
In the description of the present invention, it is to be understood that the terms "longitudinal", "lateral", "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", and the like, indicate orientations or positional relationships based on those shown in the drawings, are merely for convenience of description of the present invention, and do not indicate or imply that the referenced devices or elements must have a particular orientation, be constructed and operated in a particular orientation, and thus, are not to be construed as limiting the present invention.
The above-described embodiments are merely illustrative of the preferred embodiments of the present invention, and do not limit the scope of the present invention, and various modifications and improvements of the technical solutions of the present invention can be made by those skilled in the art without departing from the spirit of the present invention, and the technical solutions of the present invention are within the scope of the present invention defined by the claims.
Claims (10)
1. A kind controlling means is advanced to liquid chromatogram pulsed for nuclide separation which characterized in that: comprises the steps of (a) preparing a mixture of a plurality of raw materials,
a box body (1);
the input piece is arranged on one outer side wall of the box body (1), the output end of the input piece is communicated with the box body (1), the input piece is provided with an air inlet end and a liquid inlet end, and the air inlet end and the liquid inlet end work in a linkage mode;
the output piece is arranged on the other outer side wall of the box body (1) far away from the input piece, the input end of the output piece is communicated with the box body (1), the output piece is provided with a first liquid outlet end and a second liquid outlet end, and the first liquid outlet end and the second liquid outlet end work in a linkage mode;
the control piece is arranged outside the box body (1) and is used for controlling the opening and closing of the air inlet end, the liquid inlet end, the first liquid outlet end and the second liquid outlet end;
the monitoring piece is arranged in the box body (1), is used for monitoring the height of the solution in the box body (1), and is electrically connected with the control piece.
2. The pulsed sample injection control device for liquid chromatography of nuclide separation as in claim 1, characterized in that: the control piece includes a control panel (2), the rigid coupling has first relay (3) on the input piece, control panel (2) with first relay (3) electric connection, first relay (3) control the inlet end with during the output intercommunication of input piece, the feed liquor end with the output of input piece is closed, first relay (3) control the inlet end with during the output of input piece is closed, the feed liquor end with the output intercommunication of input piece.
3. The pulsed liquid chromatography sample injection control device for nuclide separation as defined in claim 2, characterized in that: the output piece is fixedly connected with a second relay (4), the control panel (2) is electrically connected with the second relay (4), the second relay (4) controls the first liquid outlet end to be communicated with the input end of the output piece, the second liquid outlet end is closed with the input end of the output piece, and the second relay (4) controls the first liquid outlet end to be communicated with the input end of the output piece when the first liquid outlet end is closed with the input end of the output piece.
4. The pulsed sample injection control device for liquid chromatography of nuclide separation as in claim 1, characterized in that: the input member include with input three-way valve (5) of box (1) lateral wall rigid coupling, the play liquid end of input three-way valve (5) with communicate in box (1), the inlet end of input three-way valve (5) passes through intake pipe (6) and outside air intercommunication, the feed liquor end of input three-way valve (5) has primary sample cell (8) through feed liquor pipe (7) intercommunication.
5. The pulsed sample injection control device for liquid chromatography of nuclide separation as in claim 4, characterized in that: the output piece include with output three-way valve (9) of box (1) lateral wall rigid coupling, output three-way valve (9) feed liquor end with communicate in box (1), the first play liquid end of output three-way valve (9) has primary sample backward flow pond (11) through first drain pipe (10) intercommunication, the second play liquid end of output three-way valve (9) has secondary sample backward flow pond (13) through second drain pipe (12) intercommunication.
6. The pulsed sample injection control device for liquid chromatography of nuclide separation as in claim 5, characterized in that: the outer wall rigid coupling of box (1) has peristaltic pump (14), peristaltic pump (14) are used for the drive intake pipe (6) conveying gas, peristaltic pump (14) are used for the drive feed liquor pipe (7) first drain pipe (10) second drain pipe (12) transport solution.
7. The pulsed sample injection control device for liquid chromatography used in nuclide separation as in claim 2, characterized in that: the monitoring part comprises a liquid level sensor (15) fixedly connected with the inner wall of the box body (1), and the liquid level sensor (15) is electrically connected with the control panel (2).
8. The pulsed sample injection control device for liquid chromatography used in nuclide separation as in claim 2, characterized in that: the outer wall of the box body (1) is fixedly connected with a display screen (16), and the display screen (16) is electrically connected with the control panel (2).
9. The control method of the pulsed injection control device for the liquid chromatogram for nuclide separation is based on the pulsed injection control device for the liquid chromatogram for nuclide separation as claimed in claim 1, and is characterized in that: the operation steps comprise:
s1, determining an initial position: starting the control part and the monitoring part, communicating the air inlet end of the input part with the box body (1), and communicating the first liquid outlet end of the output part with the box body (1);
s2, setting the operation time: setting the communication time of the air inlet end of the input element and the box body (1) to be T1, setting the communication time of the liquid inlet end of the input element and the box body (1) to be T2, and setting the communication time of the first liquid outlet end of the output element and the box body (1) to be T3;
s3, feeding liquid into the box body (1): the control piece works, after the air inlet end of the input piece is communicated with the box body (1) for T1, the liquid inlet end of the input piece is communicated with the box body (1), and after the air inlet end of the input piece is communicated for T2, the input piece stops working;
s4, draining liquid by the box body (1): the monitoring part monitors that the solution in the box body (1) rises to a certain height and then feeds back the solution to the control part, and after the control part controls the first liquid outlet end of the output part to be communicated with the box body (1) for T3, the second liquid outlet end of the output part is communicated with the box body (1);
s5, resetting the device: the monitoring part monitors the solution in the box body (1) to descend to a certain height and then feeds back the solution to the control part, the control part controls the air inlet end of the input part to be communicated with the inside of the box body (1), and the first liquid outlet end of the output part is communicated with the inside of the box body (1).
10. The use method of the pulsed sample injection control device for the liquid chromatography of nuclide separation as to claim 9, characterized in that: in step S2, time T3 is less than time T2.
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| CN211013651U (en) * | 2019-07-30 | 2020-07-14 | 广西壮族自治区农业科学院 | Sampling device for liquid on-line monitoring |
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| JP2013504756A (en) * | 2010-06-25 | 2013-02-07 | コリア ユニバーシティ リサーチ アンド ビジネス ファウンデーション | Multi-function selection valve, multi-function fully automatic liquid chromatography apparatus including the same, and sample analysis method using the same |
| CN105612424A (en) * | 2013-07-10 | 2016-05-25 | 伟德泰有限公司 | Liquid chromatography apparatus for fast measuring |
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