CN217084832U - Three-dimensional liquid chromatography separation system - Google Patents
Three-dimensional liquid chromatography separation system Download PDFInfo
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- CN217084832U CN217084832U CN202220895604.7U CN202220895604U CN217084832U CN 217084832 U CN217084832 U CN 217084832U CN 202220895604 U CN202220895604 U CN 202220895604U CN 217084832 U CN217084832 U CN 217084832U
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Abstract
The utility model discloses a three-dimensional liquid chromatography separation system relates to liquid chromatography separation technical field, and its technical scheme main points are: including the first solvent device that connects gradually, first delivery pump and sample injector, the second solvent device that connects gradually, second delivery pump and first three-way valve, first chromatographic column, the second chromatographic column, the detector, the component is collected the piece, the output of detector is connected with the input that the component was collected the piece, still include first flow path selection valve, second flow path selection valve, third flow path selection valve, fourth flow path selection valve, third chromatographic column and the third solvent device that connects gradually, third delivery pump and second three-way valve. The utility model discloses well each dimension chromatogram can realize that relative separation is independent, mutual noninterference, and arbitrary dimension chromatographic column can realize gradient or isocratic drip washing as required, and overall structure is simple, and separation efficiency is high.
Description
Technical Field
The utility model relates to a liquid chromatography separation technical field, more specifically say, it relates to a three-dimensional liquid chromatography separation system.
Background
The sample systems of rare earth mineral samples, irradiated nuclear fuel and the like contain a large amount of uranium matrixes and fission products with a large content of element types and a small amount of element types, such as rare earth elements, the properties of the fission nuclides are very similar, and the target component is one or more fission nuclides. The system is complex, the matrix content of the sample is high, the difference between the target element and the matrix is large, and the impurity elements with similar target element properties are more. Certain target components of the sample are difficult to separate out components to be detected for analysis by adopting one-dimensional liquid chromatography and even two-dimensional liquid chromatography, and a three-dimensional liquid chromatography system is invented for solving the separation and analysis of the sample.
At present, the multidimensional liquid chromatography improves the separation capacity by increasing the number of separation stages and the number of chromatographic columns, and generally, the first chromatographic column is responsible for primary separation, and the latter chromatographic column is responsible for further separation, so that the target component is separated from the complex component. Compared with the common one-dimensional high performance liquid chromatography, the multidimensional liquid chromatography has stronger separation capability and system flexibility, thereby solving the problem of separation and analysis of complex system samples. However, the existing multidimensional liquid chromatography system has a relatively complex structure and a large number of chromatographic columns. For example, chinese patent publication No. CN109557194A discloses a three-dimensional liquid chromatography system, which uses a serial mode and a plurality of enrichment column arrays, but is not suitable for separation and extraction of one or more target components in rare earth mineral samples and irradiated nuclear fuel samples.
Therefore, how to design a three-dimensional liquid chromatography separation system capable of overcoming the above defects is a problem which is urgently needed to be solved at present.
SUMMERY OF THE UTILITY MODEL
For solving the not enough among the prior art, the utility model aims at providing a three-dimensional liquid chromatography piece-rate system, can effectual realization complex component sample's separation, simple structure, classification efficiency is high.
The above technical purpose of the present invention can be achieved by the following technical solutions: a three-dimensional liquid chromatography separation system comprises a first solvent device, a first delivery pump, a sample injector, a second solvent device, a second delivery pump, a first three-way valve, a first chromatographic column, a second chromatographic column, a detector and a component collecting piece, wherein the first solvent device, the first delivery pump and the sample injector are sequentially connected;
the output end of the sample injector is connected with the input end of a first chromatographic column, the output end of the first chromatographic column is connected with the liquid inlet of a first flow path selection valve, the waste liquid port of the first flow path selection valve is externally connected with a corresponding waste liquid pipe and a corresponding waste liquid collector, the first liquid outlet of the first flow path selection valve is connected with the first liquid inlet of a second flow path selection valve, and the liquid outlet of the second flow path selection valve is connected with the input end of a detector;
the second liquid outlet of the first flow path selection valve is connected with the other input end of the first three-way valve, the output end of the first three-way valve is connected with the input end of the second chromatographic column, the output end of the second chromatographic column is connected with the liquid inlet of the third flow path selection valve, the waste liquid port of the third flow path selection valve is externally connected with a corresponding waste liquid pipe and a waste liquid collector, and the first liquid outlet of the third flow path selection valve is connected with the second liquid inlet of the second flow path selection valve;
and a second liquid outlet of the third flow path selection valve is connected with the other input end of the second three-way valve, an output end of the second three-way valve is connected with an input end of a third chromatographic column, an output end of the third chromatographic column is connected with a liquid inlet of a fourth flow path selection valve, a liquid outlet of the fourth flow path selection valve is connected with a third liquid inlet of the second flow path selection valve, and a waste liquid port of the fourth flow path selection valve is externally connected with a corresponding waste liquid pipe and a waste liquid collector.
Further, the first flow path selector valve, the second flow path selector valve, and the third flow path selector valve are each provided with at least three different flow paths.
Further, the first flow path selection valve, the second flow path selection valve and the third flow path selection valve are all ten-way valves.
Further, the fourth flow path selection valve is provided with at least two different flow paths.
Further, the fourth flow path selection valve is a ten-way valve.
Further, the fourth flow path selection valve is a two-position six-way valve.
Further, the component collecting member is a fraction collector or a manual collecting device.
Further, the first delivery pump, the second delivery pump and the third delivery pump are any one of a quaternary gradient pump, a binary gradient pump and an isocratic pump.
Further, the sample injector is a manual sample injector or an automatic sample injector.
Further, the detector is an ultraviolet detector, a diode array detector or a mass spectrometer.
Compared with the prior art, the utility model discloses following beneficial effect has:
1. the utility model provides a pair of two-dimensional liquid chromatography separation system, first dimension is responsible for separating out the target component from a large amount of base members, cut into the chromatographic column in back, first chromatographic column continues to separate, cut the target component that gets into again after the second chromatographic column separation of second dimension and get into third chromatographic column and carry out further separation and purification, each dimension chromatogram can realize that relative separation is independent in the system, mutual noninterference, and arbitrary dimension chromatographic column can realize gradient or isocratic drip washing as required, overall structure is simple, separation efficiency is high;
2. the utility model discloses can be used to the separation and purification of the complicated component of organic and inorganic chemicals, simple structure, degree of automation is high.
Drawings
The accompanying drawings, which are included to provide a further understanding of the embodiments of the invention and are incorporated in and constitute a part of this application, illustrate embodiment(s) of the invention and together with the description serve to explain the principles of the invention. In the drawings:
fig. 1 is a schematic view of the overall structure in an embodiment of the present invention;
fig. 2 is a schematic connection diagram of one-dimensional operation in the embodiment of the present invention;
fig. 3 is a schematic connection diagram of two-dimensional operation in an embodiment of the present invention;
fig. 4 is a schematic connection diagram of three-dimensional operation in the embodiment of the present invention.
Reference numbers and corresponding part names in the drawings:
101. a first solvent device; 102. a first delivery pump; 103. a sample injector; 104. a first chromatographic column; 105. a first flow path selector valve; 106. a second flow path selector valve; 107. a detector; 108. a component collection member; 109. a second solvent device; 110. a second delivery pump; 111. a first three-way valve; 112. a second chromatography column; 113. a third flow path selector valve; 114. a third solvent device; 115. a third delivery pump; 116. a second three-way valve; 117. a third chromatographic column; 118. and a fourth flow path selector valve.
Detailed Description
To make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail below with reference to the following examples and drawings, and the exemplary embodiments and descriptions thereof of the present invention are only used for explaining the present invention, and are not intended as limitations of the present invention.
It will be understood that when an element is referred to as being "secured to" or "disposed on" another element, it can be directly on the other element or be indirectly connected to the other element. When an element is referred to as being "connected to" another element, it can be directly or indirectly connected to the other element.
It will be understood that the terms "length," "width," "upper," "lower," "front," "rear," "left," "right," "vertical," "horizontal," "top," "bottom," "inner," "outer," and the like are used in an orientation or positional relationship indicated in the drawings for convenience in describing the invention and to simplify the description, and are not intended to indicate or imply that the device or element so referred to must have a particular orientation, be constructed and operated in a particular orientation, and thus should not be construed as limiting the invention.
Furthermore, the terms "first", "second" and "first" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include one or more of that feature. In the description of the present invention, "a plurality" means two or more unless specifically limited otherwise.
Example (b): a three-dimensional liquid chromatography separation system, as shown in fig. 1, includes a first solvent device 101, a first transfer pump 102, a sample injector 103, a second solvent device 109, a second transfer pump 110, a first three-way valve 111, a first chromatography column 104, a second chromatography column 112, a detector 107, a component collecting member 108, a first flow path selection valve 105, a second flow path selection valve 106, a third flow path selection valve 113, a fourth flow path selection valve 118, a third chromatography column 117, a third solvent device 114, a third transfer pump 115, and a second three-way valve 116.
The first solvent device 101, the first delivery pump 102 and the sample injector 103 are sequentially connected, the output end of the sample injector 103 is connected with the input end of the first chromatographic column 104, the output end of the first chromatographic column 104 is connected with the liquid inlet of the first flow path selection valve 105, the waste liquid port of the first flow path selection valve 105 is externally connected with a corresponding waste liquid pipe and a waste liquid collector, the first liquid outlet of the first flow path selection valve 105 is connected with the first liquid inlet of the second flow path selection valve 106, and the liquid outlet of the second flow path selection valve 106 is connected with the input end of the detector 107. The output of the detector 107 is connected to the input of a component collector 108.
The second solvent device 109, the second delivery pump 110 and the first three-way valve 111 are sequentially connected, the second liquid outlet of the first flow path selection valve 105 is connected with the other input end of the first three-way valve 111, the output end of the first three-way valve 111 is connected with the input end of the second chromatographic column 112, the output end of the second chromatographic column 112 is connected with the liquid inlet of the third flow path selection valve 113, the waste liquid port of the third flow path selection valve 113 is externally connected with a corresponding waste liquid pipe and a waste liquid collector, and the first liquid outlet of the third flow path selection valve 113 is connected with the second liquid inlet of the second flow path selection valve 106;
the third solvent device 114, the third transfer pump 115 and the second three-way valve 116 are sequentially connected, a second liquid outlet of the third flow path selection valve 113 is connected with another input end of the second three-way valve 116, an output end of the second three-way valve 116 is connected with an input end of the third chromatographic column 117, an output end of the third chromatographic column 117 is connected with a liquid inlet of a fourth flow path selection valve 118, a liquid outlet of the fourth flow path selection valve 118 is connected with a third liquid inlet of the second flow path selection valve 106, and a waste liquid port of the fourth flow path selection valve 118 is externally connected with a corresponding waste liquid pipe and a waste liquid collector.
In the present embodiment, each of the first flow path selector valve 105, the second flow path selector valve 106, and the third flow path selector valve 113 is provided with at least three different flow paths, and each of the first flow path selector valve 105, the second flow path selector valve 106, and the third flow path selector valve 113 is a ten-way valve. The fourth flow path selector valve 118 is provided with at least two different flow paths, and the fourth flow path selector valve 118 is a two-position six-way valve; the fourth flow path selector valve 118 may be a ten-way valve.
The three-way valve, the six-way valve, the ten-way valve and the like in the system are connecting components, the ten-way valve in the system is provided with a common outlet or inlet, the selection function of the flow path can be realized through software control, and other flow paths are completely blocked after one flow path is selected by the valve.
The utility model provides a three-dimensional liquid chromatography separation system contains three kinds of operational mode: one-dimensional mode, two-dimensional mode, and three-dimensional mode.
As shown in fig. 2, one-dimensional equilibrium mode: when the first chromatographic column 104 of the one-dimensional system needs to be balanced, the eluent from the first transfer pump 102 flows into the first chromatographic column 104 through the sample injector 103, reaches the liquid inlet of the first flow path selection valve 105, flows out through the waste liquid port, and flows into the waste liquid. The eluent flow path is:
one-dimensional sample separation mode: when the one-dimensional system needs to separate a sample, the eluent from the first delivery pump 102 passes through the sample injector 103, is brought into the first chromatographic column 104, then flows into the inlet of the first flow path selection valve 105, flows into the first inlet of the second flow path selection valve 106 after flowing out through the first outlet, and enters the detector 107 and the component collecting element 108 after flowing out through the outlet of the second flow path selection valve 106. The flow paths through which the target component passes are:
the whole system balance can be carried out by the sample loading mode when only one dimension is used.
As shown in fig. 3, two-dimensional equilibrium mode: in two dimensions, each chromatographic column can be balanced independently. The first chromatographic column 104 is balanced: the eluate from the first transfer pump 102 flows into the first column 104 through the sample injector 103, reaches the inlet of the first channel selector valve 105, and flows out through the waste liquid port into the waste liquid. The eluent flow path is:
when the second chromatographic column 112 is in equilibrium, the liquid from the second transfer pump 110 flows into the second chromatographic column 112 through the first three-way valve 111, flows into the liquid inlet of the third flow path selector valve 113, flows out through the waste liquid port, and enters the waste liquid. The eluent flow path is:
the positions of the valves are all switched to the waste liquid port when the two-dimensional balance mode is balanced.
Two-dimensional sample separation mode: when a two-dimensional system needs to separate a sample, the sample enters the first chromatographic column 104 through the sample injector 103, then flows into the liquid inlet of the first flow path selection valve 105, passes through the position of the switching valve to the second liquid outlet of the first flow path selection valve 105, enters the first three-way valve 111, passes through the second chromatographic column 112, enters the liquid inlet of the third flow path selection valve 113, exits from the liquid outlet of the third flow path selection valve 113, enters the second liquid inlet of the second flow path selection valve 106, exits through the liquid outlet of the second flow path selection valve 106, and enters the detector 107 and the component collection device. The route followed by the target component is:
because the ten-way valve can be switched at any time, when the ten-way valve starts an experiment, the chromatographic columns are not switched in series through switching, and the function of a full two-dimensional liquid phase can be realized. If only certain components are required to enter two dimensions, the two-dimensional chromatographic column can be continuously balanced before the sample enters the two dimensions, and the one-dimensional chromatographic column can be continuously leached or balanced after the sample enters the two dimensions.
When the linear cutting two-dimensional loading mode is adopted, the determination can be carried out according to the condition that the sample is separated in one dimension. The method comprises the steps of working in one dimension in advance, knowing the approximate time of a target component coming out of a one-dimensional chromatographic column, utilizing valve switching to select a flow path, linearly cutting the target component into a two-dimensional chromatographic column, and continuously separating under the pushing of a two-dimensional pump leacheate. The sample enters the first chromatographic column 104 through the sample injector 103, the first chromatographic column 104 separates the sample by controlling the position of the liquid outlet of the first flow path selection valve 105, and the sample (or the whole sample) is cut into the two-dimensional system for a certain period of time as required. Specifically, the sample enters the first chromatographic column 104 through the sample injector 103, the first chromatographic column 104 performs separation, the unnecessary part is discharged through the waste liquid port of the first flow path selection valve 105, the necessary part of the sample enters the two-dimensional space through the second liquid outlet of the first flow path selection valve 105, and the sample enters the second chromatographic column 112 through the first three-way valve 111. The first flow selector valve 105 returns to the waste port position after the sample is cut into the time period. If there is still a desired sample in the first chromatographic column 104, the sample can be collected manually. After further separation by the second chromatography column 112, the sample entering the two-dimensional column enters the detector 107 and the component collecting member 108 through the third flow path selection valve 113 and the second flow path selection valve 106, and a target product is obtained. The eluent flow path is:
as shown in fig. 4, the three-dimensional balance mode: in three dimensions, each chromatographic column can be balanced independently.
The first chromatographic column 104 is balanced: the eluate from the first transfer pump 102 flows into the first column 104 through the sample injector 103, reaches the inlet of the first channel selector valve 105, and flows out through the waste liquid port into the waste liquid. The eluent flow path is:
when the second chromatographic column 112 is in equilibrium, the liquid from the second transfer pump 110 flows into the second chromatographic column 112 through the first three-way valve 111, flows into the liquid inlet of the third flow path selector valve 113, flows out through the waste liquid port, and enters the waste liquid. The eluent flow path is:
the positions of the valves are all switched to when the two-dimensional balance mode is balancedA waste liquid port.
When the third column 117 is in equilibrium, the liquid from the third transfer pump 115 flows into the third column 117 through the second three-way valve 116, flows into the inlet of the fourth flow path selector valve 118, flows out through the waste liquid port, and enters the waste liquid. The specific flow path is as follows:
and the positions of the valves are switched to the waste liquid port when the three-dimensional balance mode is balanced.
Three-dimensional sample separation mode: when a sample is separated by the three-dimensional system, the sample enters the first chromatographic column 104 through the sample injector 103, then flows into the common sample inlet of the first flow path selection valve 105, is subjected to position switching through the switching valve, enters the first three-way valve 111, passes through the second chromatographic column 112, enters the liquid inlet of the third flow path selection valve 113, passes through the second three-way valve 116 after exiting from the liquid outlet, enters the third chromatographic column 117, passes through the fourth flow path selection valve 118, reaches the liquid inlet of the second flow path selection valve 106, and exits from the common outlet, and enters the detector 107 and the component collection part 108. The route followed by the target component is:
similarly, the ten-way valve and the six-way valve can be switched at any time, so that the function of the full three-dimensional liquid phase can be realized by switching the valve positions at the beginning of the experiment to ensure that the chromatographic columns are not switched any more after being connected in series. If only certain target components need to enter the second dimension and the third dimension, the sample can be continuously balanced after entering the chromatographic columns with front and rear dimensions, and the sample can be continuously separated after entering the chromatographic column with the rear dimension and the chromatographic column with the front dimension. When the same linear cutting three-dimensional sample loading mode is adopted, the determination can be carried out according to the one-dimensional and two-dimensional separation conditions. When the three-dimensional mode is adopted, the two-dimensional mode can be adopted in advance, on the basis of knowing about the two-dimensional approximate coming-out time of the target component, the function of flow path selection can be carried out by utilizing the valve switching technology, the target component is cut in a linear mode, enters the three-dimensional chromatographic column, and is continuously separated under the pushing of three-dimensional pump eluent.
Specifically, the sample enters the first chromatographic column 104 through the sample injector 103 under the driving of the eluent supplied by the first transfer pump 102, the first chromatographic column 104 performs separation, an unnecessary part is discharged through the waste liquid port of the first flow path selection valve 105, a required part of the sample is discharged through the first flow path selection valve 105 to the second liquid outlet by controlling, the sample enters two dimensions through the first three-way valve 111, the first flow path selection valve 105 returns to the waste liquid port after the sample is cut into a time period, and if the required sample still exists in the first chromatographic column 104, the sample can be collected at the waste liquid port in a manual manner. The sample entering the first three-way valve 111 enters the second chromatographic column 112 for further separation under the action of the wash supplied by the second transfer pump 110. The unnecessary part is discharged through the waste liquid port of the third flow path selection valve 113, the required part of the sample enters the second three-way valve 116 by controlling the first flow path selection valve 105 to the liquid outlet, the liquid outlet of the third flow path selection valve 113 returns to the waste liquid port after the sample is cut in for a period of time, the sample enters the third chromatographic column 117 under the push of the three-dimensional third transfer pump 115 to be further separated, the separated sample enters the fourth flow path selection valve 118 and then enters the second flow path selection valve 106 through the liquid outlet, and finally enters the detector 107 and the component collection element 108, so that the target component is obtained. The eluent flow path is:
in this embodiment, the component collecting member 108 employs a fraction collector or a manual collecting device. Further, the first transfer pump 102, the second transfer pump 110, and the third transfer pump 115 are any one of a quaternary gradient pump, a binary gradient pump, and an isocratic pump. And the injector 103 is a manual injector or an auto injector. In addition, the detector 107 may be selected from an ultraviolet detector, a diode array detector, or a mass spectrometer.
The working principle is as follows: the first dimension is responsible for separating the target components from a large number of matrixes, the target components are cut into the following chromatographic columns, the first chromatographic column 104 is continuously separated, the second chromatographic column 112 of the second dimension is separated, the cut target components enter the third chromatographic column 117 for further separation and purification, the relative separation of the chromatographic columns of all dimensions in the system is independent and not interfered with each other, and the chromatographic columns of any dimension can realize gradient or isocratic leaching according to requirements, so that the whole structure is simple, and the separation efficiency is high.
The above-mentioned embodiments, further detailed description of the objects, technical solutions and advantages of the present invention, it should be understood that the above description is only the embodiments of the present invention, and is not intended to limit the scope of the present invention, and any modifications, equivalent substitutions, improvements, etc. made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (10)
1. A three-dimensional liquid chromatography separation system comprises a first solvent device (101), a first delivery pump (102) and a sample injector (103) which are connected in sequence, a second solvent device (109), a second delivery pump (110) and a first three-way valve (111) which are connected in sequence, a first chromatographic column (104), a second chromatographic column (112), a detector (107) and a component collecting piece (108), wherein the output end of the detector (107) is connected with the input end of the component collecting piece (108), and the three-dimensional liquid chromatography separation system is characterized by further comprising a first flow path selection valve (105), a second flow path selection valve (106), a third flow path selection valve (113), a fourth flow path selection valve (118), a third chromatographic column (117), a third solvent device (114), a third delivery pump (115) and a second three-way valve (116) which are connected in sequence;
the output end of the sample injector (103) is connected with the input end of a first chromatographic column (104), the output end of the first chromatographic column (104) is connected with the liquid inlet of a first flow path selection valve (105), the waste liquid port of the first flow path selection valve (105) is externally connected with a corresponding waste liquid pipe and a waste liquid collector, the first liquid outlet of the first flow path selection valve (105) is connected with the first liquid inlet of a second flow path selection valve (106), and the liquid outlet of the second flow path selection valve (106) is connected with the input end of a detector (107);
a second liquid outlet of the first flow path selection valve (105) is connected with the other input end of the first three-way valve (111), the output end of the first three-way valve (111) is connected with the input end of the second chromatographic column (112), the output end of the second chromatographic column (112) is connected with a liquid inlet of a third flow path selection valve (113), a waste liquid port of the third flow path selection valve (113) is externally connected with a corresponding waste liquid pipe and a waste liquid collector, and a first liquid outlet of the third flow path selection valve (113) is connected with a second liquid inlet of the second flow path selection valve (106);
a second liquid outlet of the third flow path selection valve (113) is connected with the other input end of the second three-way valve (116), an output end of the second three-way valve (116) is connected with an input end of a third chromatographic column (117), an output end of the third chromatographic column (117) is connected with a liquid inlet of a fourth flow path selection valve (118), a liquid outlet of the fourth flow path selection valve (118) is connected with a third liquid inlet of the second flow path selection valve (106), and a waste liquid port of the fourth flow path selection valve (118) is externally connected with a corresponding waste liquid pipe and a corresponding waste liquid collector.
2. The three-dimensional liquid chromatography separation system according to claim 1, wherein the first flow path selector valve (105), the second flow path selector valve (106), and the third flow path selector valve (113) are each provided with at least three different flow paths.
3. The three-dimensional liquid chromatography separation system of claim 2, wherein the first flow path selector valve (105), the second flow path selector valve (106), and the third flow path selector valve (113) are all ten-way valves.
4. The three-dimensional liquid chromatography separation system of claim 1, wherein the fourth flow path selection valve (118) is configured with at least two different flow paths.
5. The three-dimensional liquid chromatography separation system of claim 4, wherein the fourth flow path selector valve (118) is a ten-way valve.
6. The three-dimensional liquid chromatography separation system of claim 4, wherein the fourth flow path selector valve (118) is a two-position, six-way valve.
7. A three-dimensional liquid chromatography separation system according to claim 1 wherein the component collection member (108) is a fraction collector or a manual collection device.
8. The three-dimensional liquid chromatography separation system of claim 1, wherein the first transfer pump (102), the second transfer pump (110), and the third transfer pump (115) are any one of a quaternary gradient pump, a binary gradient pump, and an isocratic pump.
9. The three-dimensional liquid chromatography separation system of claim 1, wherein the sample injector (103) is a manual sample injector or an automated sample injector.
10. A three-dimensional liquid chromatography separation system according to claim 1, wherein the detector (107) is an ultraviolet detector, a diode array detector or a mass spectrometer.
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