An injection chromatography device based on a four-column selection valve and its injection control method
Through the injection chromatography device of the four-column selection valve, the problems of high cost, high synchronousness requirements and insufficient pressure sensors in the liquid chromatography experiment were solved, and efficient and convenient chromatography column operation was achieved.
Patent Information
- Application Number
- CN202110323720.1
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2021-03-26
- Publication Date
- 2025-07-08
- Estimated Expiration
- 2041-03-26
AI Technical Summary
In the existing liquid chromatography experiments, the three-column parallel design has problems such as high cost, large pipeline volume, high synchronous requirements, and insufficient pressure sensors, resulting in low experimental efficiency and poor safety.
The injection chromatography device using a four-column selection valve, including a four-column selection valve, multiple chromatography columns, controllers and driving mechanisms, realizes the loading, flushing and bypass functions of the chromatography columns through the rotation of the valve core, and adds a pressure sensor to monitor the pressure difference in real time, simplifying software control.
It improves experimental efficiency and convenience, reduces the number of times the column is disassembled, reduces the risk of error, and achieves good process continuity and operational convenience.
Smart Images

Figure CN112946144B_ABST
Abstract
Description
Technical Field
[0001] The present invention relates to the field of chromatography devices, and particularly to a sample injection chromatography device based on a four-column selection valve and a sample injection control method therefor. Background Art
[0002] Currently, in liquid chromatography experiments, when staff conduct experiments on multiple chromatography columns, they often need to frequently disassemble and install the chromatography columns. There are many drawbacks in this process. For example, when disassembling the chromatography column, it is often easy to introduce a small amount of air bubbles into the chromatography column due to unskilled operation or accidental factors, which affects the performance and use of the column. In the prior art, a three-column parallel connection method has been adopted to solve the above problems. As Figure 1 shown, it includes a system pump 1', a sample injection valve 2', a sample pump 3', a column flow control valve 4', a first column selection valve 5', a second column selection valve 7', a third chromatography column 8', and a detector 9'. The outlet of the system pump 1' is connected to the buffer inlet of the sample injection valve 2'. The outlet of the sample pump 3' is connected to the sample inlet of the sample injection valve 2'. The column position valve 4' is a three-position four-way valve and is connected to the sample injection valve 2'. The first interface and the sixth interface of the column position valve 4' are respectively connected to the first column selection valve 5' and the second column selection valve 7'. The second interface of the column position valve 4' is connected to the detector 9'. The corresponding interfaces between the first column selection valve 5' and the second column selection valve 7' are respectively connected through three chromatography columns 8', and at least one group of corresponding interfaces are directly connected through pipelines.
[0003] However, the above design of three-column parallel connection still has deficiencies:
[0004] ① This design uses one column position valve and two column selection valves, greatly increasing the cost;
[0005] ② Existing four-column position valves can improve the cleaning efficiency, effectively protect the chromatography column, and leave a bypass cleaning pipeline, which can also reduce the risk of column disassembly. However, when using two column selection valves and one column position valve to achieve these functions, more pipelines are needed to connect different valves, which increases the extra-column volume of the pipelines. Compared with one valve, the efficiency of achieving these functions is lower;
[0006] ③The existing system has only one pressure sensor to detect the system pressure online, which can protect the chromatography column. However, due to the lack of a second pressure sensor after the column, the pressure difference applied to the chromatography packing cannot be measured, so the overpressure alarm cannot be set in real time. Nevertheless, overpressure protection is provided for the packing. This design requires two column selection valves. The connection between a certain chromatography column and the column selection holes on the two column selection valves must follow a certain arrangement rule, which is generally controlled by software and is difficult to change after being determined. When switching between chromatography columns or between a chromatography column and a direct connection, the software must control the rotors of the two column selection valves to rotate simultaneously so that their respective column selection slots are almost simultaneously connected to the corresponding column selection holes / direct connection holes. This process has high requirements for synchronization and accuracy. The software program is relatively complex and has a low error tolerance rate.
[0007] Therefore, to solve the above problems, a sample injection chromatography device based on a four-column selection valve and its sample injection control method are now needed. Summary of the Invention
[0008] In view of the above, it is necessary to provide a sample injection chromatography device based on a four-column selection valve and its sample injection control method, which can realize sample loading, flushing, and bypass of the column, and does not require frequent replacement of the chromatography column, greatly improving the efficiency and convenience of the experiment. The technical solutions provided by the present invention are as follows:
[0009] On the one hand, the present invention provides a sample injection chromatography device based on a four-column selection valve, including a plurality of chromatography columns, and,
[0010] A four-column selection valve for selecting different chromatography columns, which includes a valve body in the shape of a disc and a valve core arranged on the valve body. Among them,
[0011] The valve body is provided with a sample loading valve interface at the center and ten auxiliary interfaces that are equidistant from the sample loading valve interface and are distributed in a circular pattern. The auxiliary interfaces include a bypass interface, a detector interface, and eight column interfaces. Among them, the sample loading valve interface is connected to an external sample loading valve, the bypass interface is connected to an external mobile phase storage container, the detector interface is connected to an external detector, and the column interfaces are respectively connected to the two ends of the chromatography column in a one-to-one correspondence.
[0012] The valve core is provided with four through grooves. The first through groove is used to connect the detector interface with any one of the auxiliary interfaces. The second through groove is used to connect two adjacent auxiliary interfaces. The third through groove is used to connect one auxiliary interface and another auxiliary interface that is separated from it by two auxiliary interfaces. The fourth through groove is used to connect one auxiliary interface and another auxiliary interface that is separated from it.
[0013] A controller and a driving mechanism. Under the control of the controller, the driving mechanism can drive the valve core to rotate relative to the valve body.
[0014] Further, the chromatography column includes a first chromatography column, a second chromatography column, a third chromatography column, and a fourth chromatography column, and the column interfaces include a first positive column interface and a first negative column interface, a second positive column interface and a second negative column interface, a third positive column interface and a third negative column interface, and a fourth positive column interface and a fourth negative column interface.
[0015] Further, the first positive column interface, the second positive column interface, the third positive column interface, and the fourth positive column interface respectively correspond to the sample injection ends of the first chromatography column, the second chromatography column, the third chromatography column, and the fourth chromatography column;
[0016] The first negative column interface, the second negative column interface, the third negative column interface, and the fourth negative column interface respectively correspond to the sample output ends of the first chromatography column, the second chromatography column, the third chromatography column, and the fourth chromatography column.
[0017] On the other hand, the present invention provides a sample injection control method for the sample injection chromatography device as described above, which controls the sample injection of any chromatography column in the sample injection chromatography device. The sample injection end of the target chromatography column is pre-connected to the target positive column interface, and the sample output end of the target chromatography column is connected to the target negative column interface;
[0018] The sample injection control method includes: controlling the rotation of the valve core of the four-column selection valve until the sample injection valve interface communicates with the target positive column interface through the through groove on the valve core, and the target negative column interface communicates with the detector interface through another through groove, and then opening the sample injection valve for sample injection.
[0019] Further, the four-column selection valve of the sample injection chromatography device includes a sample injection valve interface and a detector interface. The control method further includes controlling the system flushing, including:
[0020] Controlling the rotation of the valve core of the four-column selection valve until the sample injection valve interface communicates with the detector interface, and controlling the detector interface to be connected to the detector, and then opening the sample injection valve for system flushing.
[0021] Further, the four-column selection valve of the sample injection chromatography device includes a bypass interface and a sample injection valve interface. The control method further includes controlling the mobile phase bypass, including:
[0022] Controlling the rotation of the valve core of the four-column selection valve until the sample injection valve interface communicates with the bypass interface, and controlling the bypass interface to be connected to the carrier container containing the required bypass mobile phase, and then opening the sample injection valve for mobile phase bypass.
[0023] Further, the sample injection control method is based on the sample injection chromatography device as described in claims 1-3, and performs function switching control according to the following different working positions:
[0024] When the spool of the four-column selection valve is in the first working position, the sample injection valve interface of the four-column selection valve is communicated with the detector interface, and the sample injection valve is opened for system flushing;
[0025] When the spool is in the second working position, the sample injection valve interface is connected to the first positive column interface of the four-column selection valve, the first positive column interface is connected to the injection end of the first chromatographic column, the sample outlet end of the first chromatographic column is communicated with the first negative column interface of the four-column selection valve, and the first negative column interface is communicated with the detector interface. The sample injection valve is opened for sample injection and detection of the first chromatographic column;
[0026] When the spool is in the third working position, the sample injection valve interface is connected to the second positive column interface of the four-column selection valve, the second positive column interface is connected to the injection end of the second chromatographic column, the sample outlet end of the second chromatographic column is communicated with the second negative column interface of the four-column selection valve, and the second negative column interface is communicated with the detector interface. The sample injection valve is opened for sample injection and detection of the second chromatographic column;
[0027] When the spool is in the fourth working position, the sample injection valve interface is connected to the third positive column interface of the four-column selection valve, the third positive column interface is connected to the injection end of the third chromatographic column, the sample outlet end of the third chromatographic column is communicated with the third negative column interface of the four-column selection valve, and the third negative column interface is communicated with the detector interface. The sample injection valve is opened for sample injection and detection of the third chromatographic column;
[0028] When the spool is in the fifth working position, the sample injection valve interface is connected to the fourth positive column interface of the four-column selection valve, the fourth positive column interface is connected to the injection end of the fourth chromatographic column, the sample outlet end of the fourth chromatographic column is communicated with the fourth negative column interface of the four-column selection valve, and the fourth negative column interface is communicated with the detector interface. The sample injection valve is opened for sample injection and detection of the fourth chromatographic column;
[0029] When the spool is in the sixth working position, the sample injection valve interface of the four-column selection valve is communicated with the bypass interface, and the sample injection valve is opened for mobile phase bypass.
[0030] The present invention has the following advantages:
[0031] a) It is not necessary to disassemble the chromatographic column multiple times, which improves the experimental efficiency and has good process continuity;
[0032] b) Using one column selection valve instead of multiple valves can avoid errors caused by asynchronous switching of multiple valves;
[0033] c) The connection rule between the chromatographic column and the valve body interface is simple and fixed, and the software program is simple and clear, not easy to make mistakes, and the operation is convenient. Description of the Drawings
[0034] To more clearly illustrate the technical solutions in the embodiments of the present invention, the following briefly introduces the accompanying drawings required for description in the embodiments. Obviously, the accompanying drawings in the following description are only some embodiments of the present invention. For those of ordinary skill in the art, without creative efforts, other accompanying drawings can be obtained based on these drawings.
[0035] Figure 1 It is a schematic connection diagram of each component in the three-column parallel method in the prior art;
[0036] Figure 2 It is a valve body structure diagram provided by an embodiment of the present invention;
[0037] Figure 3 It is a spool structure diagram provided by an embodiment of the present invention;
[0038] Figure 4 It is a schematic diagram of the first working position provided by an embodiment of the present invention;
[0039] Figure 5 It is a schematic diagram of the second working position provided by an embodiment of the present invention;
[0040] Figure 6 It is a schematic diagram of the third working position provided by an embodiment of the present invention;
[0041] Figure 7 It is a schematic diagram of the fourth working position provided by an embodiment of the present invention;
[0042] Figure 8 It is a schematic diagram of the fifth working position provided by an embodiment of the present invention;
[0043] Figure 9 It is a schematic diagram of the sixth working position provided by an embodiment of the present invention.
[0044] Among them, the reference numerals include: 1-valve body, 11-bypass interface, 12-sampling valve interface, 13-detector interface, 2-spool. Detailed implementation manners
[0045] In order to enable those skilled in the art to better understand the solution of the present invention, and to more clearly understand the purpose, technical solution and its advantages of the present invention, the technical solutions in the embodiments of the present invention will be clearly and completely described below in conjunction with specific embodiments and with reference to the accompanying drawings. It should be noted that the implementation manners not illustrated or described in the drawings are forms known to those of ordinary skill in the art. In addition, although this text may provide examples containing parameters with specific values, it should be understood that the parameters do not necessarily have to be exactly equal to the corresponding values, but may approximate the corresponding values within an acceptable error tolerance or design constraint. Obviously, the described embodiments are only a part of the embodiments of the present invention, rather than all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative efforts shall fall within the protection scope of the present invention. In addition, the terms "comprising" and "having" in the description and claims of the present invention, and any variations thereof, are intended to cover non-exclusive inclusion. For example, a process, method, apparatus, product or device that comprises a series of steps or units does not necessarily have to be limited to those steps or units clearly listed, but may include other steps or units not clearly listed or inherent to these processes, methods, products or devices.
[0046] In one embodiment of the present invention, a sample injection chromatography device based on a four-column selection valve is provided, as Figure 2 , 3 shown. The sample injection chromatography device includes a plurality of chromatography columns, a four-column selection valve, a controller and a driving mechanism. The chromatography columns are connected to the four-column selection valve. The four-column selection valve includes a valve body 1 and a valve core 2. Under the control of the controller, the driving mechanism drives the valve core 2 to rotate relative to the valve body 1 to achieve the functions of sample loading on the chromatography column, system flushing, and mobile phase bypass.
[0047] Specifically, in an embodiment of the present invention, there are four chromatography columns in the sample injection chromatography device, namely the first chromatography column, the second chromatography column, the third chromatography column, and the fourth chromatography column (hereinafter simply referred to as column C1, column C2, column C3, and column C4); the four-column selection valve is an eleven-hole six-channel valve, and there is a sample injection valve interface 12 and ten auxiliary interfaces on the valve body 1. The ten auxiliary interfaces include a bypass interface 11 (hereinafter simply referred to as W), a detector interface 13 (hereinafter simply referred to as Out), and eight column interfaces. The eight column interfaces include a first positive column interface and a first negative column interface, a second positive column interface and a second negative column interface, a third positive column interface and a third negative column interface, a fourth positive column interface and a fourth negative column interface (hereinafter simply referred to as C1+ and C1-, C2+ and C2-, C3+ and C3-, C4+ and C4-); there are four through grooves on the valve core 2. The first through groove (hereinafter simply referred to as L1) is used to connect the detector interface 13 to any one of the auxiliary interfaces, the second through groove (hereinafter simply referred to as L2) is used to connect two adjacent auxiliary interfaces, the third through groove (hereinafter simply referred to as L3) is used to connect one auxiliary interface and another auxiliary interface separated by two auxiliary interfaces from it, and the fourth through groove (hereinafter simply referred to as L4) is used to connect one auxiliary interface and another auxiliary interface separated from it.
[0048] The sample injection valve interface 12 is connected to an external sample injection valve, the bypass interface 11 is connected to an external mobile phase storage container, the detector interface 13 is connected to an external detector, and the column interfaces are respectively connected to the two ends of the chromatography column in a one-to-one correspondence. Specifically, the first positive column interface, the second positive column interface, the third positive column interface, and the fourth positive column interface respectively correspond to the sample injection ends of the first chromatography column, the second chromatography column, the third chromatography column, and the fourth chromatography column, and the first negative column interface, the second negative column interface, the third negative column interface, and the fourth negative column interface respectively correspond to the sample output ends of the first chromatography column, the second chromatography column, the third chromatography column, and the fourth chromatography column.
[0049] It should be noted that, in this embodiment, as Figure 2 shown, the valve body 1 is in a disc shape, the sample injection valve interface 12 is arranged at the center of the valve body 1, and the ten auxiliary interfaces are equidistant from the sample injection valve interface 12 and are circumferentially distributed at equal intervals on the inner circumference of the valve body 1.
[0050] In an embodiment of the present invention, the connection modes of L1, L2, L3, and L4 are as follows:
[0051] (1) The groove L1 connects the mobile phase introduced from the sample injection valve interface 12 to Out to achieve the system flushing function, or the groove L1 connects the mobile phase introduced from the sample injection valve interface 12 to W to achieve the mobile phase bypass function;
[0052] (2) The groove L1 connects the mobile phase introduced from the sample injection valve interface 12 to C1+, and the groove L3 connects C1- to Out, so as to enable the detector to detect the sample loading condition of column C1;
[0053] (3) The groove L1 connects the mobile phase introduced from the sample injection valve interface 12 to C2+, and the groove L2 connects C2- to Out, so as to enable the detector to detect the sample loading condition of column C2;
[0054] (4) The groove L1 connects the mobile phase introduced from the sample injection valve interface 12 to C3+, and the groove L3 connects C3- to Out, so as to enable the detector to detect the sample loading condition of column C3;
[0055] (5) The groove L1 connects the mobile phase introduced from the sample injection valve interface 12 to C4+, and the groove L4 connects C4- to Out, so as to enable the detector to detect the sample loading condition of column C4;
[0056] It should be noted that the number, sequence, and distribution positions of the above interfaces are only for illustrative purposes and do not limit the protection scope of the present invention.
[0057] In an embodiment of the present invention, under the control of the controller, the driving mechanism drives the valve core 2 of the four-column selection valve to rotate relative to the valve body 1 to realize the above groove connection method, so that the sample injection chromatography device has the following six working positions:
[0058] (1) As Figure 4 shown, the sample injection chromatography device is in the first working position, and the mobile phase introduced from the sample injection valve interface 12 directly flows to Out to realize the system flushing function;
[0059] (2) As Figure 5 shown, the sample injection chromatography device is in the second working position, and the mobile phase introduced from the sample injection valve interface 12 flows through L1 to C1+, passes through column C1 to C1-, and then flows through L3 to Out to realize the sample loading function of column C1;
[0060] (3) As Figure 6 shown, the sample injection chromatography device is in the third working position, and the mobile phase introduced from the sample injection valve interface 12 flows through L1 to C2+, passes through column C2 to C2-, and then flows through L2 to Out to realize the sample loading function of column C2;
[0061] (4) As Figure 7 shown, the sample injection chromatography device is in the fourth working position, and the mobile phase introduced from the sample injection valve interface 12 flows through L1 to C3+, passes through column C3 to C3-, and then flows through L3 to Out to realize the sample loading function of column C3;
[0062] (5) As Figure 8 shown, the sample injection chromatography device is in the fifth working position. The mobile phase introduced from the sample injection valve interface 12 flows through L1 to C4+, then through column C4 to C4-, and then through L4 to Out, realizing the function of loading and sampling on column C4;
[0063] (6) As Figure 9 shown, the sample injection chromatography device is in the sixth working position. The mobile phase introduced from the sample injection valve interface 12 directly flows to W, realizing the function of bypassing the mobile phase;
[0064] In addition, in an embodiment of the present invention, a first pressure sensor and a second pressure sensor are further provided in the sample injection chromatography device. The first pressure sensor is used to detect the system pressure to protect the chromatography column. The second pressure sensor is arranged behind the chromatography column. By detecting the pressure difference applied to the chromatography packing, an alarm threshold is preset to realize overpressure alarm prompt, so as to protect the packing from overpressure.
[0065] In an embodiment of the present invention, a test usually used for a group of multiple sample sequences is provided, and it can also be used for testing a single type of multi-component sample; first, system flushing is required. The four-column selection valve is switched to Figure 4 state through software, and then column flushing is carried out respectively. The four-column selection valve is switched to Figure 5 , Figure 6 , Figure 7 , Figure 8 respectively through software to perform forward column flushing on columns 1, 2, 3, and 4. The system flushing status is detected by a detector. After the column flushing is completed, loading and sampling are started. The four-column selection valve is switched to Figure 5 , Figure 6 , Figure 7 , Figure 8 respectively through software to perform forward column sampling, and the sampling status is detected by a detector.
[0066] In an embodiment of the present invention, a sample injection control method for the sample injection chromatography device as described above is provided, which controls the sampling of any chromatography column in the sample injection chromatography device. The injection end of the target chromatography column is pre-connected to the target positive column interface, and the outlet end of the target chromatography column is connected to the target negative column interface;
[0067] The sample injection control method includes: controlling the rotation of the valve core 2 of the four-column selection valve until the sample injection valve interface 12 is communicated with the target positive column interface through the through groove on the valve core 2, and the target negative column interface is communicated with the detector interface 13 through another through groove, and then opening the sample injection valve for sample injection.
[0068] In one embodiment of the present invention, a sample injection control method is provided, which also controls system flushing, including: controlling the rotation of the valve core 2 of the four-column selection valve until the sample injection valve interface 12 is communicated with the detector interface 13, controlling the detector interface 13 to be connected to the detector, and then opening the sample injection valve to perform system flushing.
[0069] In one embodiment of the present invention, a sample injection control method is provided, which also controls mobile phase bypass, including: controlling the rotation of the valve core 2 of the four-column selection valve until the sample injection valve interface 12 is communicated with the bypass interface 11, controlling the bypass interface 11 to be connected to a carrier container containing the required bypass mobile phase, and then opening the sample injection valve to perform mobile phase bypass.
[0070] In one embodiment of the present invention, a sample injection control method is provided, which can perform function switching control according to the following different working positions through the above sample injection chromatography device:
[0071] When the valve core 2 of the four-column selection valve is in the first working position, the sample injection valve interface 12 of the four-column selection valve is communicated with the detector interface 13, and the sample injection valve is opened to perform system flushing;
[0072] When the valve core 2 is in the second working position, the sample injection valve interface 12 is connected to the first positive column interface of the four-column selection valve, the first positive column interface is connected to the injection end of the first chromatography column, the outlet end of the first chromatography column is communicated with the first negative column interface of the four-column selection valve, the first negative column interface is communicated with the detector interface 13, and the sample injection valve is opened to perform sample injection and detection of the first chromatography column;
[0073] When the valve core 2 is in the third working position, the sample injection valve interface 12 is connected to the second positive column interface of the four-column selection valve, the second positive column interface is connected to the injection end of the second chromatography column, the outlet end of the second chromatography column is communicated with the second negative column interface of the four-column selection valve, the second negative column interface is communicated with the detector interface 13, and the sample injection valve is opened to perform sample injection and detection of the second chromatography column;
[0074] When the valve core 2 is in the fourth working position, the sample injection valve interface 12 is connected to the third positive column interface of the four-column selection valve, the third positive column interface is connected to the injection end of the third chromatography column, the outlet end of the third chromatography column is communicated with the third negative column interface of the four-column selection valve, the third negative column interface is communicated with the detector interface 13, and the sample injection valve is opened to perform sample injection and detection of the third chromatography column;
[0075] When the spool 2 is in the fifth working position, the sample injection valve interface 12 is connected to the fourth positive column interface of the four-column selection valve, the fourth positive column interface is connected to the sample injection end of the fourth chromatography column, the sample outlet end of the fourth chromatography column is communicated with the fourth negative column interface of the four-column selection valve, and the fourth negative column interface is communicated with the detector interface 13. Open the sample injection valve to perform sample injection detection on the fourth chromatography column;
[0076] When the spool 2 is in the sixth working position, the sample injection valve interface 12 of the four-column selection valve is communicated with the bypass interface 11. Open the sample injection valve to perform mobile phase bypass.
[0077] The idea of the embodiment of this sample injection control method belongs to the same idea as the working process of the sample injection chromatography device in the above embodiment. The entire content of the embodiment of the above sample injection chromatography device is incorporated into the embodiment of this sample injection control method by way of full reference, and will not be elaborated here.
[0078] The present invention utilizes the process of combining a column position valve with a switching valve for chromatography, which has relatively good advantages compared with single-column connection. During the experiment, after finishing an experiment on one chromatography column, it is not necessary to remove the chromatography column and replace it with another one. Only need to connect four different chromatography columns to the four-column selection valve, and by changing the column position in the software, it will automatically switch to the second, third, and fourth chromatography columns, and the second experiment can be directly carried out on another chromatography column. Moreover, the four-column position valve also has bypass and flushing functions. Such operation has more obvious advantages: ① It is not necessary to often remove the chromatography column from the chromatography system. When removing the chromatography column, it is often easy to introduce a small amount of air bubbles into the chromatography column due to unskilled operation or accidental factors, which will affect the performance and use of the column; ② By using the method of four-column parallel connection, during the process exploration of process development, the chromatography columns can be cleaned online during the preparation stage before the experiment, and there is no need to replace them during the experiment, which has good continuity and convenience in process development and greatly improves the efficiency and convenience of the experiment; ③ The added four-column position valve control valve can realize column bypass, positive sample injection and reverse cleaning, bringing convenience to column operation.
[0079] The above are only the preferred embodiments of the present invention, and do not limit its patent scope accordingly. Any equivalent structure or equivalent process transformation made by using the content of the specification and drawings of the present invention, directly or indirectly applied in other related technical fields, shall be similarly included in the patent protection scope of the present invention.
Claims
1. A sample injection chromatography device based on a four-column selection valve, characterized in that, including a plurality of chromatography columns, and, a four-column selection valve for selecting different chromatography columns, which includes a valve body (1) in the shape of a disc and a valve core (2) provided on the valve body (1), wherein, the valve body (1) is provided with a sample loading valve interface (12) at the center, and ten auxiliary interfaces equidistant from the sample loading valve interface (12) and distributed in a circular pattern. The auxiliary interfaces include a bypass interface (11), a detector interface (13), and eight column interfaces. Among them, the sample loading valve interface (12) is connected to an external sample loading valve, the bypass interface (11) is connected to an external mobile phase reservoir, the detector interface (13) is connected to an external detector, and the column interfaces are respectively connected to the two ends of the chromatography columns in a one-to-one correspondence. The eight column interfaces include C1+ and C1-, C2+ and C2-, C3+ and C3-, C4+ and C4-. The detector interface is Out, and the bypass interface is W. Among them, C2-, C4-, C1-, and C4+ are distributed between Out and W, and C1+, C2-, C3-, and C3+ are distributed between Out and W; the first chromatography column to the fourth chromatography column are C1 to C4 respectively, C1+, C2+, C3+, and C4+ respectively correspond to the injection ends of C1, C2, C3, and C4, and C1-, C2-, C3-, and C4- respectively correspond to the sampling ends of C1, C2, C3, and C4; the valve core is provided with four through grooves. The first through groove is used to connect the detector interface (13) to any one of the auxiliary interfaces, the second through groove is used to connect two adjacent auxiliary interfaces, the third through groove is used to connect one auxiliary interface and another auxiliary interface separated by two auxiliary interfaces, and the fourth through groove is used to connect one auxiliary interface and another auxiliary interface separated by it. The first through groove to the fourth through groove are L1 to L4 respectively; a controller and a driving mechanism. Under the control of the controller, the driving mechanism can drive the valve core (2) to rotate relative to the valve body (1). The sample injection chromatography device has the following six working positions: when the sample injection chromatography device is in the first working position, the mobile phase introduced from the sample loading valve interface 12 directly flows to Out to realize the system flushing function; when the sample injection chromatography device is in the second working position, the mobile phase introduced from the sample loading valve interface 12 flows through L1 to C1+, through column C1 to C1-, and then through L3 to Out to realize the column C1 loading and sampling function; when the sample injection chromatography device is in the third working position, the mobile phase introduced from the sample loading valve interface 12 flows through L1 to C2+, through column C2 to C2-, and then through L2 to Out to realize the column C2 loading and sampling function; when the sample injection chromatography device is in the fourth working position, the mobile phase introduced from the sample loading valve interface 12 flows through L1 to C3+, through column C3 to C3-, and then through L3 to Out to realize the column C3 loading and sampling function; The sample injection chromatography device is in the fifth working position. The mobile phase introduced from the sample injection valve interface 12 flows through L1 to C4+, then through column C4 to C4-, and then through L4 to Out, realizing the sample loading function of column C4. The sample injection chromatography device is in the sixth working position. The mobile phase introduced from the sample injection valve interface 12 directly flows to W, realizing the mobile phase bypass function.
2. The sample injection chromatography device according to claim 1, wherein It further includes a first pressure sensor, which is used to detect the system pressure to protect the chromatography column.
3. The sample injection chromatography device according to claim 1, characterized in that, It further includes a second pressure sensor, which is arranged behind the chromatography column. By detecting the pressure difference applied to the chromatography packing, the alarm threshold is preset to realize the overpressure alarm prompt, so as to protect the packing from overpressure.
4. A sample injection control method for the sample injection chromatography device as described in claim 1, characterized in that, Control the sample loading of any chromatography column in the sample injection chromatography device. First, connect the injection end of the target chromatography column to the target positive column interface, and connect the outlet end of the target chromatography column to the target negative column interface. The sample loading control method includes: controlling the rotation of the valve core (2) of the four-column selection valve until the sample injection valve interface (12) is connected to the target positive column interface through the through groove on the valve core (2), and the target negative column interface is connected to the detector interface (13) through another through groove, and then opening the sample injection valve for sample loading.
5. The sample injection control method according to claim 4, characterized in that The four-column selection valve of the sample injection chromatography device includes a sample injection valve interface (12) and a detector interface (13). The control method further includes controlling the system flushing, including: Controlling the rotation of the valve core (2) of the four-column selection valve until the sample injection valve interface (12) is connected to the detector interface (13), and controlling the detector interface (13) to be connected to the detector, and then opening the sample injection valve for system flushing.
6. The sample injection control method according to claim 4, wherein, The four-column selection valve of the sample injection chromatography device includes a bypass interface (11) and a sample injection valve interface (12). The control method further includes controlling the mobile phase bypass, including: Controlling the rotation of the valve core (2) of the four-column selection valve until the sample injection valve interface (12) is connected to the bypass interface (11), and controlling the bypass interface (11) to be connected to the carrier container containing the mobile phase to be bypassed, and then opening the sample injection valve for mobile phase bypass.
7. The sample injection control method according to claim 4, wherein The sample injection control method is based on the sample injection chromatography device described in claims 1-3, and performs function switching control according to the following different working positions: When the valve core (2) of the four-column selection valve is in the first working position, the sample injection valve interface (12) of the four-column selection valve is connected to the detector interface (13), and the sample injection valve is opened for system flushing. When the valve core (2) is in the second working position, the sample injection valve interface (12) is connected to the first positive column interface of the four-column selection valve, the first positive column interface is connected to the injection end of the first chromatography column, the outlet end of the first chromatography column is connected to the first negative column interface of the four-column selection valve, the first negative column interface is connected to the detector interface (13), and the sample injection valve is opened for sample loading and detection of the first chromatography column. When the valve core (2) is in the third working position, the sample injection valve interface (12) is connected to the second positive column interface of the four-column selection valve. The second positive column interface is connected to the sample injection end of the second chromatographic column. The sample outlet end of the second chromatographic column is communicated with the second negative column interface of the four-column selection valve. The second negative column interface is communicated with the detector interface (13). Open the sample injection valve to perform sample injection detection on the second chromatographic column; When the valve core (2) is in the fourth working position, the sample injection valve interface (12) is connected to the third positive column interface of the four-column selection valve. The third positive column interface is connected to the sample injection end of the third chromatographic column. The sample outlet end of the third chromatographic column is communicated with the third negative column interface of the four-column selection valve. The third negative column interface is communicated with the detector interface (13). Open the sample injection valve to perform sample injection detection on the third chromatographic column; When the valve core (2) is in the fifth working position, the sample injection valve interface (12) is connected to the fourth positive column interface of the four-column selection valve. The fourth positive column interface is connected to the sample injection end of the fourth chromatographic column. The sample outlet end of the fourth chromatographic column is communicated with the fourth negative column interface of the four-column selection valve. The fourth negative column interface is communicated with the detector interface (13). Open the sample injection valve to perform sample injection detection on the fourth chromatographic column; When the valve core (2) is in the sixth working position, the sample injection valve interface (12) of the four-column selection valve is communicated with the bypass interface (11). Open the sample injection valve to perform mobile phase bypass.
Citation Information
Patent Citations
Multi-column-position column valve and chromatography system achieving multi-column positive and reverse flow and bypass function on basis of multi-column-position column valve
CN104455559A
Chromatographic system for implementing double-column back-and-forth flowing and bypass functions based on single seven-way valve
CN204275566U
Sample injection chromatography device based on four-column selector valve
CN214473049U