CN108445120B - Binary gradient solvent conveying system for chromatograph - Google Patents
Binary gradient solvent conveying system for chromatograph Download PDFInfo
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- CN108445120B CN108445120B CN201810114137.8A CN201810114137A CN108445120B CN 108445120 B CN108445120 B CN 108445120B CN 201810114137 A CN201810114137 A CN 201810114137A CN 108445120 B CN108445120 B CN 108445120B
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- G01—MEASURING; TESTING
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- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
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Abstract
The invention discloses a binary gradient solvent conveying system for a chromatograph, which is characterized in that: the system include pump head A, pump head B and diverter valve (1), the casing of diverter valve (1) on be provided with a plurality of infusion mouths and two imbibition mouths, these two imbibition mouths link to each other with first stock solution bottle (2) and second stock solution bottle (3) through the pipeline respectively, still be provided with the liquid outlet on the casing of diverter valve (1), then be provided with the case in diverter valve (1), the case can rotate for the casing of diverter valve (1), still be provided with a plurality of interface channel (4) on the case, just the tip and the infusion mouth of interface channel (4), imbibition mouth and liquid outlet phase-match still are provided with the sealing ring at the tip of interface channel (4). The binary gradient solvent conveying system for the chromatograph has the advantages of simple structure, easiness in realization and high flow precision.
Description
Technical Field
The invention relates to a solvent conveying system, in particular to a binary gradient solvent conveying system for a chromatograph.
Background
The high performance liquid chromatograph is one of the most widely used analytical instruments in the analytical chemistry field, and the liquid delivery system is the driving force of the liquid chromatographic separation analysis, and the performance of the high performance liquid chromatograph directly determines the result of the separation analysis. If the flow of the infusion system is inaccurate and discontinuous, a reliable result cannot be obtained, and even the analysis cannot be completed in serious cases. In order to ensure continuous delivery of high-pressure flow, infusion systems typically employ two or more pump heads to alternately deliver the same fluid in series or in parallel, and ball seat-type check valves are required at the inlet and outlet of the pump heads to ensure one-way fluid flow in the pump heads and prevent backflow.
The micro-nano liquid chromatography is the extension and expansion of high performance liquid chromatography in a low flow direction, and has wide application in the field of separation and analysis of biological samples due to extremely low solvent consumption, sample consumption and dilution effect. For the micro-nano liquid chromatography infusion system, the volume of fluid required by one analysis experiment is generally dozens of microliters, so that a single pump head with a large pump cavity volume can be used for delivering one fluid. In order to enable the fluid to flow in the pump head in a one-way mode, ball seat type one-way valves can be arranged at the inlet and the outlet of the pump head respectively in a mode of referring to a conventional liquid chromatography infusion system, but because the flow rate used by micro-nano liquid chromatography is extremely low, the one-way valve at the outlet of the pump head can be opened by the fluid with a longer time and a larger volume when the fluid is infused under high pressure, so that the volume of the effective fluid for analysis is reduced. At the same time, the flow accuracy is also significantly affected because the required flow level is on the same order of magnitude as the leakage level of the inlet check valve (tens to hundreds of nanoliters per minute). Therefore, how to ensure the accurate and effective transfusion of the micro-nano liquid chromatography transfusion system is one of the main problems to be solved for developing the micro-nano transfusion system.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provides a binary gradient solvent conveying system for a chromatograph, which has the advantages of simple structure, easy realization and high flow precision.
The technical solution of the invention is as follows: a binary gradient solvent conveying system for a chromatograph is characterized in that: the system include pump head A, pump head B and diverter valve 1, diverter valve 1's casing on be provided with a plurality of transfusion mouth and two imbibition mouths, these two imbibition mouths link to each other with first stock solution bottle 2 and second stock solution bottle 3 through the pipeline respectively, still be provided with the liquid outlet on diverter valve 1's casing, then be provided with the case in diverter valve 1, the case can rotate for diverter valve 1's casing, still be provided with a plurality of interface channel 4 on the case, just interface channel 4's tip and transfusion mouth, imbibition mouth and liquid outlet phase-match.
Infusion mouth and liquid outlet be two, these liquid mouths and imbibition mouth circumference evenly distributed on diverter valve 1's casing altogether, mark 1 to No. 6 liquid mouths with all six liquid mouths according to clockwise direction in proper order, wherein 1, No. 4 liquid mouths are the infusion mouth, 2, No. 3 liquid mouths are the liquid outlet, 5, No. 6 liquid mouths are the imbibition mouth, pump head A links to each other with No. 1 liquid mouth, pump head B links to each other with No. 4 liquid mouths, No. 2 liquid mouths and No. 3 liquid mouths simultaneously with mix three-way 5's two pipeline intercommunication, No. 5 liquid mouths pass through the pipeline and link to each other with second stock solution bottle 3, No. 6 liquid mouths pass through the pipeline and link to each other with first stock solution bottle 2.
The number of the transfusion ports and the number of the liquid outlets are two, the shell of the switching valve 1 is also provided with four plugging liquid ports which are matched with the end part of the connecting channel 4, the liquid ports and the liquid suction ports are uniformly distributed on the circumference of the shell of the switching valve 1, all ten liquid ports are marked as liquid ports 1 to 10 in sequence in the clockwise direction, the liquid ports 1 and 6 are liquid infusion ports, the liquid ports 2 and 5 are liquid outlet ports, the liquid ports 7 and 10 are liquid suction ports, the liquid ports 3, 4, 8 and 9 are blocking liquid ports, the pump head A is connected with the liquid port 1, the pump head B is connected with the liquid port 6, the liquid port 2 and the liquid port 5 are simultaneously communicated with two pipelines of a mixing tee joint 5, the liquid port 7 is connected with the second liquid storage bottle 3 through a pipeline, the liquid port 6 is connected with the first liquid storage bottle 2 through a pipeline, and all the blocking liquid ports are provided with blocking heads 6.
The transfusion mouth be two, the liquid outlet be one, these liquid mouths distribute on diverter valve 1's casing with the imbibition mouth jointly, mark 1 to No. 5 liquid mouths with all five liquid mouths according to clockwise in proper order, wherein 1, No. 3 liquid mouths are the transfusion mouth, No. 2 liquid mouths are the liquid outlet, 4, No. 5 liquid mouths are the imbibition mouth, pump head A links to each other with No. 1 liquid mouth, pump head B links to each other with No. 3 liquid mouths, No. 2 liquid mouths link to each other with the play liquid pipeline, No. 4 liquid mouths pass through the pipeline and link to each other with second stock solution bottle 3, No. 5 liquid mouths pass through the pipeline and link to each other with first stock solution bottle 2.
Compared with the prior art, the invention has the following advantages:
the binary gradient solvent conveying system for the chromatograph can save a check valve structure on a conventional pump head on the premise of ensuring the unidirectional flow of fluid, avoids the leakage of the check valve under extremely low flow (dozens to hundreds of nanoliters per minute), obviously improves the accuracy of a transfusion system under the flow of micro nanoliters, and has the advantages of simple structure, easy realization and the like. Therefore, the method has multiple advantages, is particularly suitable for popularization and application in the field, and has very wide market prospect.
Drawings
FIG. 1 is a schematic view of an infusion state according to an embodiment of the present invention.
FIG. 2 is a schematic view of a fluid-imbibing state according to an embodiment of the invention.
FIG. 3 is a schematic view of a second infusion state in accordance with an embodiment of the present invention.
FIG. 4 is a schematic view of a second imbibition state of an embodiment of the invention.
FIG. 5 is a schematic view showing the liquid-absorbing state of the pump head A in the third embodiment of the present invention.
FIG. 6 is a schematic view of the infusion state of the pump head A in the third embodiment of the present invention.
FIG. 7 is a schematic view showing the liquid-absorbing state of pump head B in the third embodiment of the present invention.
FIG. 8 is a schematic view of the infusion state of pump head B in the third embodiment of the present invention.
FIG. 9 is a schematic view of the simultaneous infusion state of pump head A and pump head B in the third embodiment of the present invention.
Detailed Description
The following description will explain embodiments of the present invention with reference to the accompanying drawings. As shown in fig. 1 to 9: the utility model provides a binary gradient solvent conveying system for chromatograph, it includes pump head A, pump head B and diverter valve 1, is provided with a plurality of transfusion mouths and two imbibition mouths on diverter valve 1's casing to these two imbibition mouths link to each other with first stock solution bottle 2 and second stock solution bottle 3 through the pipeline respectively, still are provided with the liquid outlet on diverter valve 1's casing, are connected with out the liquid pipeline on the liquid outlet, then are provided with the case in diverter valve 1, the case can rotate for diverter valve 1's casing, still be provided with a plurality of interface channel 4 on the case, just interface channel 4's tip and transfusion mouth, imbibition mouth and liquid outlet phase-match.
Example one
As shown in fig. 1 and 2, the switching valve 1 used in the binary gradient solvent delivery system of example 1 is a uniform six-hole three-channel two-state switching valve.
No. 1, No. 4 liquid mouths on the casing of the switching valve 1 are respectively connected with outlets of a pump head A and a pump head B which are responsible for conveying different fluids through pipelines made of stainless steel or polymer materials, No. 2 and No. 3 liquid mouths are respectively connected with two inlets of a mixing tee joint 5, and No. 5 and No. 6 liquid mouths are respectively connected with liquid storage bottles of a fluid B (a second liquid storage bottle 3) and a fluid A (a first liquid storage bottle 2).
When the infusion system is in an infusion state (as shown in figure 1), the inner core of the switching valve 1 acts to connect a plurality of connecting channels 4 on the inner core with different liquid ports, so that the liquid ports 1 and 2, the liquid ports 3 and 4 and the liquid ports 5 and 6 are connected. Then the plunger rods in the pump head A and the pump head B move forwards to compress the fluid in the pump cavity, so that the fluid flows out from the outlet of the pump head, the fluid in the pump head A enters the mixing tee joint 5 through the No. 1 fluid port and the No. 2 fluid port, the fluid in the pump head B enters the mixing tee joint 5 through the No. 4 fluid port and the No. 3 fluid port, and the two fluids are mixed in the mixing tee joint and then flow out through the outlets of the mixing tee joint, so that the transfusion operation is realized; the mixing tee joint 5 can ensure that two solvents are output simultaneously, and can also realize the mixing of the two solvents by utilizing a cavity in the center of the tee joint, so that the proportion of the flowing mixed fluid is uniform;
when the infusion system is in a liquid suction state (as shown in figure 2), the inner core of the switching valve 1 acts to enable the plurality of connecting channels 4 on the inner core to be connected with different liquid ports, and connection of the liquid ports 1 and 6, the liquid ports 2 and 3 and the liquid ports 4 and 5 is ensured. Then the plunger rods in the pump head A and the pump head B move backwards, negative pressure occurs in the pump cavity, the fluid A in the first liquid storage bottle 2 enters the pump head A through the No. 6 liquid opening and the No. 1 liquid opening, and the fluid B in the second liquid storage bottle 3 enters the pump head B through the No. 5 liquid opening and the No. 4 liquid opening, so that liquid suction operation is realized. Meanwhile, the No. 2 liquid port is connected with the No. 3 liquid port, so that the fluid pressure outside the transfusion system can be maintained, and the influence of sudden change of the pressure on other subsequent system components is avoided.
Example two
As shown in fig. 3 and 4, the switching valve 1 used in the binary gradient solvent delivery system of example 2 is a uniform ten-hole five-channel two-state switching valve.
No. 1 and No. 6 liquid ports on a shell of the switching valve 1 are respectively connected with outlets of a pump head A and a pump head B which are responsible for conveying different fluids through pipelines made of stainless steel or polymer materials, No. 2 and No. 5 liquid ports are respectively connected with two inlets of a mixing tee joint 5, No. 7 and No. 10 liquid ports are respectively connected with a liquid storage bottle of a fluid B (a second liquid storage bottle 3) and a liquid storage bottle of a fluid A (a first liquid storage bottle 2), and No. 3, No. 4, No. 8 and No. 9 liquid ports are provided with plugging heads 6 (screwed plugs);
when the infusion system is in an infusion state (as shown in fig. 3), the inner core of the switching valve 1 is actuated to connect a plurality of connecting channels 4 on the inner core with different liquid ports, so as to ensure that the liquid ports 1 and 2, the liquid ports 3 and 4, the liquid ports 5 and 6, the liquid ports 7 and 8, and the liquid ports 9 and 10 are connected. Then the plunger rods in the pump head A and the pump head B move forwards to compress the fluid in the pump cavity, so that the fluid flows out from the outlet of the pump head, the fluid in the pump head A enters the mixing tee joint 5 through the No. 1 fluid port and the No. 2 fluid port, the fluid in the pump head B enters the mixing tee joint 5 through the No. 6 fluid port and the No. 5 fluid port, and the two fluids are mixed in the mixing tee joint and then flow out through the outlets of the mixing tee joint, so that the transfusion operation is realized; the mixing tee joint 5 can ensure that two solvents are output simultaneously, and can also realize the mixing of the two solvents by utilizing a cavity in the center of the tee joint, so that the proportion of the flowing mixed fluid is uniform;
when the transfusion system is in a liquid suction state (as shown in figure 4), the inner core of the switching valve 1 is actuated, so that a plurality of connecting channels 4 on the inner core are connected with different liquid ports, and the connection of liquid ports 1 and 10, liquid ports 2 and 3, liquid ports 4 and 5, liquid ports 6 and 7 and liquid ports 8 and 9 is ensured. Then the plunger rods in the pump head A and the pump head B move backwards, negative pressure occurs in the pump cavity, the fluid A in the first liquid storage bottle 2 enters the pump head A through the No. 10 liquid opening and the No. 1 liquid opening, and the fluid B in the second liquid storage bottle 3 enters the pump head B through the No. 7 liquid opening and the No. 6 liquid opening, so that liquid suction operation is realized. Meanwhile, the No. 2 liquid port is connected with the No. 3 liquid port, and the No. 4 liquid port is connected with the No. 5 liquid port, so that the blocking head 6 at the upper liquid delivery port can maintain the fluid pressure outside the liquid delivery system, and the influence of the sudden change of the pressure on other subsequent system components is avoided.
EXAMPLE III
As shown in fig. 5-9, the switching valve used in the binary gradient solvent delivery system of example 3 was a non-uniform five-hole, single-channel, five-state switching valve.
Wherein, the included angles between the connecting line of the No. 1 liquid port and the center of the switching valve 1 and the connecting lines of the No. 2, 3, 4 and 5 liquid ports and the center of the switching valve are respectively 45 degrees, 90 degrees, 180 degrees and 270 degrees. No. 1, No. 3 liquid mouths on the casing of the switching valve 1 are respectively connected with outlets of a pump head A and a pump head B which are responsible for conveying different fluids through pipelines made of stainless steel or polymer materials, a No. 2 liquid mouth is connected with an outlet pipeline of the infusion pump, and No. 5 and No. 4 liquid mouths are respectively connected with liquid storage bottles of a fluid A (a first liquid storage bottle 2) and a fluid B (a second liquid storage bottle 3).
When the infusion system is in a liquid suction state of a pump head A (as shown in figure 5), the inner core of the switching valve 1 acts to enable the plurality of connecting channels 4 on the inner core to be connected with different liquid ports, connection of the liquid ports 1 and 5 is guaranteed, then the plunger rod in the pump head A moves backwards, negative pressure occurs in the pump cavity, and fluid A enters the pump head A from the first liquid storage bottle 2 through the liquid ports 5 and 1, so that liquid suction operation of the pump head A is achieved.
When the transfusion system is in a transfusion state of the pump head A (as shown in fig. 6), the inner core of the switching valve 1 acts to connect the No. 1 liquid port with the No. 2 liquid port, the plunger rod in the pump head A moves forwards, and fluid in the pump cavity flows out from the outlet of the pump head A and is directly discharged through the liquid outlet pipeline after passing through the No. 1 liquid port and the No. 2 liquid port, so that the transfusion operation of the pump head A is realized.
Similarly, the liquid suction and transfusion operations of the pump head B are realized through the sequential matching action of the inner core and the pump head B. (as shown in FIGS. 7 and 8)
When the infusion system is in the state of infusion by pump head A, B at the same time (as shown in fig. 9), the connection channel 4 in the switching valve 1 can make the liquid ports 1, 2 and 3 connected at the same time, at this time, the fluid in the pump head A, B passes through the liquid ports 1 and 3, then is mixed at the liquid port 2, and finally is discharged through the liquid outlet pipeline at the same time, so that the infusion operation at the same time of the pump head a and the pump head B is realized.
Claims (2)
1. A binary gradient solvent conveying system for a chromatograph is characterized in that: the system comprises a pump head A, a pump head B and a switching valve (1), wherein a plurality of infusion ports and two liquid suction ports are arranged on a shell of the switching valve (1), the two liquid suction ports are respectively connected with a first liquid storage bottle (2) and a second liquid storage bottle (3) through pipelines, a liquid outlet is also arranged on the shell of the switching valve (1), a valve core is arranged in the switching valve (1), the valve core can rotate relative to the shell of the switching valve (1), a plurality of connecting channels (4) are also arranged on the valve core, and the end parts of the connecting channels (4) are matched with the infusion ports, the liquid suction ports and the liquid outlet,
the number of the transfusion ports and the number of the liquid outlets are two, four plugging liquid ports are also arranged on the shell of the switching valve (1), and the plugging liquid ports are matched with the end part of the connecting channel (4), the liquid ports and the liquid suction ports are uniformly distributed on the circumference of a shell of the switching valve (1) together, all ten liquid ports are marked as liquid ports 1-10 in a clockwise direction, the liquid ports 1 and 6 are liquid infusion ports, the liquid ports 2 and 5 are liquid outlet ports, the liquid ports 7 and 10 are liquid suction ports, the liquid ports 3, 4, 8 and 9 are blocking liquid ports, the pump head A is connected with the liquid port 1, the pump head B is connected with the liquid port 6, the liquid port 2 and the liquid port 5 are simultaneously communicated with two pipelines of a mixing tee joint (5), the liquid port 7 is connected with a second liquid storage bottle (3) through a pipeline, the liquid port 6 is connected with a first liquid storage bottle (2) through a pipeline, and all the blocking liquid ports are provided with blocking heads (6).
2. A binary gradient solvent conveying system for a chromatograph is characterized in that: the system comprises a pump head A, a pump head B and a switching valve (1), wherein a plurality of infusion ports and two liquid suction ports are arranged on a shell of the switching valve (1), the two liquid suction ports are respectively connected with a first liquid storage bottle (2) and a second liquid storage bottle (3) through pipelines, a liquid outlet is also arranged on the shell of the switching valve (1), a valve core is arranged in the switching valve (1), the valve core can rotate relative to the shell of the switching valve (1), a plurality of connecting channels (4) are also arranged on the valve core, and the end parts of the connecting channels (4) are matched with the infusion ports, the liquid suction ports and the liquid outlet,
the number of the liquid outlets is one, the liquid outlets and the liquid suction ports are distributed on a shell of the switching valve (1) together, all five liquid outlets are marked as liquid outlets No. 1 to No. 5 in a clockwise direction, wherein the liquid outlets No. 1 and No. 3 are liquid outlets, the liquid outlets No. 2 and No. 4 and No. 5 are liquid suction ports, the pump head A is connected with the liquid outlet No. 1, the pump head B is connected with the liquid outlet No. 3, the liquid outlet No. 2 is connected with a liquid outlet pipeline, the liquid outlet No. 4 is connected with the second liquid storage bottle (3) through a pipeline, the liquid outlet No. 5 is connected with the first liquid storage bottle (2) through a pipeline,
wherein, the included angles between the connecting line of the No. 1 liquid port and the center of the switching valve (1) and the connecting lines of the No. 2, 3, 4 and 5 liquid ports and the center of the switching valve are respectively 45 degrees, 90 degrees, 180 degrees and 270 degrees.
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| CN201810114137.8A CN108445120B (en) | 2018-02-05 | 2018-02-05 | Binary gradient solvent conveying system for chromatograph |
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| CN111812261A (en) * | 2020-07-20 | 2020-10-23 | 大连依利特分析仪器有限公司 | Multi-mode chromatography solvent management system and control method thereof |
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