Capillary chromatography column simultaneous filling apparatus

Abstract

The utility model discloses a kind of capillary chromatographic column synchronous filling instruments, it is related to chromatography technical field, capillary chromatographic column synchronous filling instrument includes: filling module and chromatographic column connector assembly, filling module is equipped with filler mouth, pressure supply interface and chromatographic column interface;Wherein, chromatographic column interface includes connecting mouth section and sealing mouth section, the inner diameter of connecting mouth section is greater than the inner diameter of sealing mouth section to form step surface at the connecting place of connecting mouth section and sealing mouth section, fixed joint includes threaded connection part and conical sealing part, threaded connection part is connected with connecting mouth section by screw thread, at least part of conical sealing part extends into sealing mouth section and conical sealing part is pressed on the inner peripheral edge of step surface.According to the capillary chromatographic column synchronous filling instrument of the utility model, long-term stable dynamic sealing can be realized under high pressure, the risk of liquid leakage is eliminated, the structure is simple and durable, the use of parts is reduced, assembly is simple, cost is reduced, and the use range is wider.

Description

Technical Field

[0001] This utility model relates to the field of chromatography technology, and in particular to a capillary column synchronous packing apparatus. Background Technology

[0002] Capillary column packing is a key pretreatment technique in liquid chromatography (LC) analysis. Its core purpose is to form a uniform and stable chromatographic separation column by packing stationary phase particles under high pressure. Currently, the mainstream packing methods mainly include two categories: gas-pressurized packing and liquid-pressurized packing. Liquid-pressurized packing offers significantly better pressure stability than gas-pressurized packing, faster packing speed, and higher packing uniformity, and is therefore considered the mainstream technology direction for future capillary column packing.

[0003] However, when using the liquid pressurized packing method for liquid chromatographs, additional sealing connectors and two-stage connectors are required. Under high pressure, it is difficult to maintain the seal between the connector and the column for a long time, which can easily lead to leakage. The connection between the column and the sealing connector requires a special two-stage connector, which is expensive. Furthermore, the device needs to be deeply integrated with the liquid chromatograph, which occupies additional instrument resources and limits its widespread application in small and medium-sized laboratories. In order to ensure the seal, many small parts are added, making assembly complex and cumbersome. Utility Model Content

[0004] This invention aims to solve at least one of the technical problems existing in the prior art. To this end, this invention proposes a capillary column synchronous packing device, which achieves both fixed installation of the chromatographic column on the packing module and reliable sealing. It can achieve long-term stable dynamic sealing under high pressure, eliminating the risk of leakage. The structure is simple and durable, reduces the number of parts, simplifies assembly, lowers costs, and has a wider range of applications.

[0005] A capillary column synchronous packing apparatus according to an embodiment of the present invention includes: a packing module and a column connector assembly. The packing module is provided with a packing port, a pressure supply port, and a column interface. The pressure supply port, the packing port, and the column interface are all connected. The column connector assembly includes a fixing connector and a column. The fixing connector is inserted into the column interface, and the column passes through the fixing connector. The column interface includes a connecting section and a sealing section. The inner diameter of the connecting section is larger than the inner diameter of the sealing section to form a stepped surface at the connection between the connecting section and the sealing section. The fixing connector includes a threaded connection portion and a tapered sealing portion. The threaded connection portion is threadedly connected to the connecting section. At least a portion of the tapered sealing portion extends into the sealing section and presses against the inner periphery of the stepped surface.

[0006] According to the capillary column synchronous packing apparatus of this utility model, the column interface is configured to include a connecting section and a sealing section. The inner diameter of the connecting section is larger than that of the sealing section to form a stepped surface at the connection between the connecting section and the sealing section. The fixing structure is configured to include a threaded connection part and a conical sealing part, so that the threaded connection part is threadedly connected to the connecting section. The threaded connection part pushes at least a portion of the conical sealing part into the sealing section, and the inner periphery of the stepped surface and the threaded connection part together squeeze the conical sealing part, so that the conical sealing part is tightly pressed against the inner periphery of the stepped surface. Thus, the fixed joint realizes the fixed installation of the column on the packing module and also achieves a reliable sealing effect. It can achieve long-term stable dynamic sealing under high pressure, eliminate the risk of leakage, has a simple and durable structure, reduces the use of parts, completely eliminates the setting of redundant joints (especially two-stage joints), simplifies assembly, reduces costs, and has a wider range of applications.

[0007] According to some embodiments of the capillary column synchronous packing apparatus of the present invention, the stepped surface is constructed as an inner conical surface, the inner diameter of the inner conical surface is set to gradually decrease from the end connected to the connecting port section to the end connected to the sealing port section, the outer peripheral wall of the conical sealing part is formed with an outer conical surface, and the outer conical surface seals against the end of the inner conical surface connected to the sealing port section.

[0008] According to some embodiments of the capillary column synchronous packing apparatus of the present invention, the angle between the outer conical surface and the axial direction of the fixed connector is smaller than the angle between the inner conical surface and the axial direction of the column interface.

[0009] According to some embodiments of the capillary column synchronous packing apparatus of the present invention, the threaded connection part and the conical sealing part are integrally formed parts; or, the threaded connection part and the conical sealing part are separate parts, and the end face of the threaded connection part abuts against the end face of the conical sealing part.

[0010] According to some embodiments of the capillary column synchronous packing apparatus of the present invention, the column connector assembly further includes an inner fixing tube, a main through hole is formed in the threaded connection part, a fixing through hole is formed in the conical sealing part, the inner diameter of the main through hole is larger than the inner diameter of the fixing through hole, and the inner fixing tube is sequentially inserted through the main through hole and the fixing through hole and clamped and fixed at the fixing through hole.

[0011] According to some embodiments of the capillary chromatography column synchronous packing apparatus of the present invention, the fixed through hole includes a guide hole section and a fixed hole section connected along the axial direction. The guide hole section is connected between the fixed hole section and the main through hole. The inner diameter of the guide hole section is constructed to gradually decrease along the direction close to the fixed hole section. The inner fixed tube is clamped and fixed at the fixed hole section.

[0012] According to some embodiments of the capillary column synchronous packing apparatus of the present invention, a packing module has a packing cavity formed therein, and the packing port and the column interface are connected through the packing cavity; wherein, the column interface is one or more; in some specific embodiments, the column interface is at least two, and at least two column interfaces are respectively connected to the packing cavity, and the column connector assembly is at least two and is installed in a one-to-one correspondence with at least two column interfaces.

[0013] According to some embodiments of the capillary chromatography column synchronous packing apparatus of the present invention, the packing module is constructed as a cubic block structure and has multiple structural surfaces. The packing port and the chromatography column interface are respectively located on two adjacent structural surfaces, and at least two structural surfaces are respectively provided with one chromatography column interface.

[0014] According to some embodiments of the present invention, the capillary column synchronous packing apparatus further includes a magnetic stirrer, wherein the packing chamber is filled with a magnetic stir bar, and the magnetic stirrer is used to drive the magnetic stir bar to stir within the packing chamber.

[0015] According to some embodiments of the present invention, the capillary column synchronous packing apparatus further includes a constant pressure pump connected to the pressure supply interface. The constant pressure pump provides pressure to the packing module through the pressure supply interface to move the packing material at the packing port toward the column interface.

[0016] According to some embodiments of the capillary column synchronous packing apparatus of the present invention, the constant pressure pump is connected to the pressure supply interface through a pressure supply pipe, the pressure supply pipe is provided with a connecting joint, the connecting joint is threadedly connected to the pressure supply interface, and the pressure supply interface is provided with a sealing ring that seals against the end face of the connecting joint.

[0017] Additional aspects and advantages of this invention will be set forth in part in the description which follows, and in part will be obvious from the description, or may be learned by practice of the invention. Attached Figure Description

[0018] The above and / or additional aspects and advantages of this utility model will become apparent and readily understood from the description of the embodiments taken in conjunction with the following drawings, in which: Figure 1 This is a schematic diagram of the structure of a capillary column synchronous packing apparatus according to an embodiment of the present invention; Figure 2 This is an exploded view of the filling module, connecting joint, and chromatographic column connector assembly according to an embodiment of the present utility model; Figure 3 The assembly of the filling module, connecting joint, and chromatographic column connector assembly according to embodiments of the present invention. Figure 1 ; Figure 4 The assembly of the filling module, connecting joint, and chromatographic column connector assembly according to embodiments of the present invention. Figure 2 ; Figure 5 The assembly of the filling module, connecting joint, and chromatographic column connector assembly according to embodiments of the present invention. Figure 3 ; Figure 6 yes Figure 5 Cross-sectional view at point AA; Figure 7 The assembly of the filling module, connecting joint, and chromatographic column connector assembly according to embodiments of the present invention. Figure 4 ; Figure 8 yes Figure 7 Cross section at BB Figure 1 (The threaded connection and the tapered seal are integrally formed). Figure 9 yes Figure 8 Enlarged view at point A; Figure 10 yes Figure 7 Cross section at BB Figure 2 (The threaded connection and the tapered seal are set separately); Figure 11 yes Figure 10 Enlarged view at point B; Figure 12 This is a schematic diagram of the structure of the packing port configured as a chromatographic column interface according to an embodiment of the present invention; Figure 13 This is a cross-sectional view of the packing port configured as a chromatographic column interface according to an embodiment of the present invention.

[0019] Figure label: 100 capillary column synchronous packing system Packing module 1, packing port 11, column interface 12, connecting section 121, sealing section 122, stepped surface 123, packing cavity 13, structural surface 14, pressure supply interface 15. The chromatographic column connector assembly 2 includes a fixed connector 21, a threaded connection 211, a main through hole 2111, a conical sealing part 212, a fixed through hole 2121, a guide hole section 21211, a fixing hole section 21212, an outer conical surface 2122, and a tightening part 213. Column 22, internal fixation tube 23, 3. Constant pressure pump, 4. Pressure supply pipe, 41. Connecting joint, 5. Sealing part, 6. Sealing gasket. Detailed Implementation

[0020] The embodiments of this utility model are described in detail below. Examples of these embodiments are shown in the accompanying drawings, wherein the same or similar reference numerals denote the same or similar elements or elements having the same or similar functions throughout. The embodiments described below with reference to the accompanying drawings are exemplary and are only used to explain this utility model, and should not be construed as limiting this utility model.

[0021] In the description of this utility model, it should be understood that the terms "center," "longitudinal," "transverse," "length," "width," "thickness," "upper," "lower," "front," "rear," "left," "right," "vertical," "horizontal," "top," "bottom," "inner," "outer," "clockwise," "counterclockwise," "axial," "radial," and "circumferential," etc., indicating the orientation or positional relationship shown in the accompanying drawings, are only for the convenience of describing this utility model and simplifying the description, and do not indicate or imply that the device or element referred to must have a specific orientation, or be constructed and operated in a specific orientation, and therefore should not be construed as a limitation of this utility model. Furthermore, features defined with "first" or "second" may explicitly or implicitly include one or more of that feature. In the description of this utility model, unless otherwise stated, "a plurality of" means two or more. In the description of this utility model, it should be noted that, unless otherwise explicitly specified and limited, the terms "installation," "connection," and "joining" should be interpreted broadly. For example, they can refer to a fixed connection, a detachable connection, or an integral connection; they can refer to a mechanical connection or an electrical connection; they can refer to a direct connection or an indirect connection through an intermediate medium; and they can refer to the internal connection of two components. Those skilled in the art can understand the specific meaning of the above terms in this utility model based on the specific circumstances.

[0022] The following is for reference. Figures 1-13The capillary column synchronous packing apparatus 100 according to an embodiment of the present invention not only realizes the fixed installation of the chromatographic column 22 on the packing module 1, but also achieves a reliable sealing function. It can achieve long-term stable dynamic sealing under high pressure, eliminate the risk of leakage, has a simple and durable structure, reduces the use of parts, is easy to assemble, reduces costs, and has a wider range of applications.

[0023] like Figures 1-13 As shown, a capillary column synchronous packing apparatus 100 according to an embodiment of the present invention includes: a packing module 1 and a column connector assembly 2.

[0024] The capillary column synchronous packing apparatus 100 is mainly used to precisely pack the stationary phase into the chromatographic column 22 to form a highly efficient separation channel. The capillary column synchronous packing apparatus 100 of this application can be used to pack various types of capillary chromatographic columns 22, such as quartz capillary columns, stainless steel capillary columns, etc.

[0025] The capillary column synchronous packing apparatus 100 includes a packing module 1 and a column connector assembly 2. The packing module 1 is used to pack the packing material and uniformly fill the interior of the chromatographic column 22. The column connector assembly 2 is used to fix the chromatographic column 22 in the packing module 1 so that the packing module 1 can fill the chromatographic column 22 and ensure sealing to prevent liquid leakage.

[0026] The filling module 1 is provided with a filling port 11, a pressure supply port 15 and a chromatographic column interface 12. The pressure supply port 15, the filling port 11 and the chromatographic column interface 12 are all connected. The chromatographic column connector assembly 2 includes a fixed connector 21 and a chromatographic column 22. The fixed connector 21 is inserted into the chromatographic column interface 12 and the chromatographic column 22 is inserted into the fixed connector 21.

[0027] Specifically, the packing port 11 is used to add packing material into the packing module 1, and the pressure supply port 15 is used to add high-pressure liquid media (such as methanol, acetonitrile, etc.) into the packing module 1 so that the packing material can be mixed with the liquid media (such as methanol, acetonitrile, etc.) to form a suspension. The pressure transmitted by the high-pressure liquid media can then fill the chromatographic column 22 with the packing material. The chromatographic column interface 12 is used to connect the chromatographic column connector assembly 2. The fixing connector 21 of the chromatographic column connector assembly 2 is adapted to the chromatographic column interface 12 so that the fixing connector 21 can be inserted into the chromatographic column interface 12, thereby realizing the insertion connection between the fixing connector 21 and the chromatographic column interface 12. The fixing connector 21 may be provided with a through hole so that the chromatographic column 22 can be inserted into the fixing connector 21 through the through hole, thereby realizing the fixed installation of the chromatographic column 22 in the packing module 1 and the packing of the chromatographic column 22. The packing port 11 and the pressure supply port 15 are both connected to the column interface 12, so that the high-pressure liquid medium can continuously enter the packing module 1 through the pressure supply port 15. Under the pressure of the high-pressure liquid medium, the packing material flows to the column interface 12 and contacts the column 22 in the column interface 12, so that the packing material is uniformly filled in the column 22, thereby achieving uniform filling of the column 22.

[0028] Furthermore, the column interface 12 includes a connecting section 121 and a sealing section 122. The inner diameter of the connecting section 121 is larger than the inner diameter of the sealing section 122 to form a stepped surface 123 at the connection between the connecting section 121 and the sealing section 122. The fixed connector 21 includes a threaded connection portion 211 and a tapered sealing portion 212. The threaded connection portion 211 is threadedly connected to the connecting section 121. At least a portion of the tapered sealing portion 212 extends into the sealing section 122 and presses against the inner periphery of the stepped surface 123.

[0029] Specifically, the connecting section 121 is used to fix the fixed connector 21, and the sealing section 122 is used to seal the fixed connector 21, preventing gaps from forming between the outer peripheral wall of the fixed connector 21 and the inner peripheral wall of the connecting section 121, which would cause liquid to leak from the gap between the column interface 12 and the fixed connector 21, affecting the packing effect of the column 22. (See attached diagram.) Figure 9As shown, the inner diameter of the connecting section 121 is larger than the inner diameter of the sealing section 122, so that a stepped surface 123 is formed at the connection between the connecting section 121 and the sealing section 122. The stepped surface 123 forms a certain angle with both the connecting section 121 and the sealing section 122, which can be any angle. The fixed joint 21 includes a threaded connection part 211 and a conical sealing part 212. The threaded connection part 211 is used to fix the connection with the connecting section 121. An external thread can be provided on the outer peripheral wall of the threaded connection part 211, and an internal thread adapted to the external thread can be provided on the inner peripheral wall of the connecting section 121. Thus, the threaded connection between the threaded connection part 211 and the connecting section 121 can be achieved by the mutual engagement of the external thread and the internal thread, thereby achieving the fixed connection between the fixed joint 21 and the chromatographic column interface 12 and preventing the fixed joint 21 and the chromatographic column interface 12 from separating or loosening.

[0030] When the threaded connection 211 and the connection port section 121 are tightened, so that the threaded connection 211 and the connection port section 121 are fastened together by the threads, at least a portion of the conical seal 212 will extend into the sealing port section 122, and the conical seal 212 will be tightly pressed against the inner periphery of the step surface 123 under the tightening force. In other words, when the threaded connection 211 is tightened, the threaded connection 211 will squeeze and push the conical seal 212, so that the conical seal 212 is in close contact with the inner periphery of the step surface 123, thereby achieving a seal between the fixed joint 21 and the sealing port section 122 and preventing liquid leakage. Since the threaded connection 211 and the connection port section 121 are fastened together, the conical seal 212 can always be tightly pressed against the inner periphery of the step surface 123 without loosening or gaps, thereby greatly improving the sealing effect and achieving long-term stable dynamic sealing under high pressure, eliminating the risk of leakage.

[0031] In practical design, such as Figure 9 As shown, the column interface 12 may also include a tightening part 213 connected to the threaded connection part 211. The tightening part 213 is the part that the user directly contacts to apply external force. The threaded connection part 211 can be tightened to the connection port section 121 by rotating the tightening part 213 to apply tightening force. That is, the threaded connection part 211 and the connection port section 121 are securely connected by the tightening part 213 to prevent the connection between the threaded connection part 211 and the connection port section 121 from loosening. After the connection is completed, the tightening part 213 is located outside the column interface 12, so that the user can disassemble the fixed connector 21 by rotating the tightening part 213 in the opposite direction to apply external force after use. This is flexible and convenient. The radial dimension of the tightening part 213 can be set to be larger than the radial dimension of the threaded connection part 211 or the connection port section 121 to form a limiting effect on the tightening part 213 and prevent the tightening part 213 from extending into the column interface 12.

[0032] It should be noted that in the prior art, the chromatographic column 22 is installed on the nut, and the nut is installed on the chromatographic column interface 12. An additional sealing connector and a two-stage connector are required on the nut. The chromatographic column 22 and the sealing connector are connected through the two-stage connector. The assembly is complicated, with many parts and expensive accessories. Moreover, the device needs to be used with a liquid chromatograph, which occupies additional instrument resources and limits its widespread application in small and medium-sized laboratories. Furthermore, under high pressure, the sealing performance between the connector and the chromatographic column 22 is difficult to maintain for a long time, and leakage problems are prone to occur. In contrast, this application achieves the fixed installation of the chromatographic column 22 on the packing module 1 by using the fixed connector 21. At the same time, it also achieves a reliable sealing effect. The structure is simple and durable, completely eliminating the setting of redundant connectors (especially the two-stage connector). The assembly is simple, the cost is reduced, and the application range is wider, which can be applied to small and medium-sized laboratories.

[0033] According to the capillary column synchronous packing apparatus 100 of this utility model embodiment, the column interface 12 is configured to include a connecting section 121 and a sealing section 122. The inner diameter of the connecting section 121 is larger than the inner diameter of the sealing section 122 to form a stepped surface 123 at the connection between the connecting section 121 and the sealing section 122. The fixing structure is configured to include a threaded connection portion 211 and a tapered sealing portion 212, such that the threaded connection portion 211 is threadedly connected to the connecting section 121. The threaded connection portion 211 pushes at least a portion of the tapered sealing portion 212 to extend into the sealing section. Within 122, the inner periphery of the stepped surface 123 and the threaded connection 211 together press against the conical sealing part 212, so that the conical sealing part 212 tightly presses against the inner periphery of the stepped surface 123. Thus, the fixed joint 21 not only realizes the fixed installation of the chromatographic column 22 on the packing module 1, but also achieves a reliable sealing effect. It can achieve long-term stable dynamic sealing under high pressure, eliminate the risk of leakage, has a simple and durable structure, reduces the use of parts, completely eliminates the setting of redundant joints (especially two-stage joints), reduces costs, and has a wider range of applications.

[0034] In some embodiments, the stepped surface 123 is configured as an inner conical surface, and the inner diameter of the inner conical surface is set to gradually decrease from the end connected to the connecting section 121 to the end connected to the sealing section 122. The outer peripheral wall of the conical sealing part 212 is formed with an outer conical surface 2122, and the outer conical surface 2122 is sealed against the end of the inner conical surface connected to the sealing section 122.

[0035] Specifically, such as Figure 9 and Figure 11 As shown, the stepped surface 123 is constructed as an inner conical surface, that is, the stepped surface 123 is inclined, as... Figure 9 and Figure 11As shown in the left-right direction, the right end of the inner conical surface is connected to the connecting section 121, and the left end of the inner conical surface is connected to the sealing section 122. The inner diameter of the inner conical surface gradually decreases from the left end to the right end, that is, the inner diameter of the inner conical surface gradually decreases from the end connected to the connecting section 121 to the end connected to the sealing section 122. An outer conical surface 2122 is formed on the outer peripheral wall of the conical sealing part 212. When the outer conical surface 2122 extends into the sealing section 122, the left end of the inner conical surface, i.e., the inner conical surface, is connected to the sealing section 122. One end connected to 122 will squeeze the outer conical surface 2122, so that the outer conical surface 2122 and the left end of the inner conical surface are tightly pressed together, thereby circumferentially sealing the fixed joint 21 and improving the sealing effect. At the same time, since the chromatographic column 22 passes through the fixed joint 21, when the outer conical surface 2122 is squeezed, the inner peripheral wall of the conical sealing part 212 will press the chromatographic column 22, thereby making the chromatographic column 22 more stably fixed in the fixed joint 21 and improving the fixation effect of the chromatographic column 22.

[0036] In some embodiments, such as Figure 9 and Figure 11 As shown, the angle between the outer conical surface 2122 and the fixed connector 21 is smaller than the angle between the inner conical surface and the column interface 12.

[0037] Therefore, when at least a portion of the conical sealing part 212 extends into the sealing port section 122, the inner conical surface can better compress the outer conical surface 2122, resulting in a better sealing effect. At the same time, it will not cause excessive obstruction to the process of the outer conical surface 2122 extending into the sealing port section 122. Furthermore, a certain gap can be formed at other places where the outer conical surface 2122 and the inner conical surface are pressed together, so as to facilitate the movement of the conical sealing part 212 and achieve dynamic sealing. The inner peripheral wall of the conical sealing part 212 will not cause excessive pressure on the chromatographic column 22, resulting in deformation of the chromatographic column 22, etc.

[0038] In some embodiments, such as Figure 8 and Figure 9 As shown, the threaded connection part 211 and the conical sealing part 212 are integrally formed parts.

[0039] In other words, the threaded connection part 211 and the conical sealing part 212 are integrated into one piece, which facilitates the manufacturing of the fixed joint 21, further reduces the number of parts, improves manufacturing efficiency, and at the same time ensures the connection strength between the threaded connection part 211 and the conical sealing part 212.

[0040] Or, such as Figure 10 and Figure 11 As shown, the threaded connection part 211 and the conical sealing part 212 are separate parts, and the end face of the threaded connection part 211 presses against the end face of the conical sealing part 212.

[0041] In other words, the threaded connection 211 and the conical seal 212 are each configured as two separate structural components. This means that if either the threaded connection 211 or the conical seal 212 is damaged, only one component can be replaced without replacing the entire fixed connector 21, reducing maintenance costs and improving maintenance convenience. Furthermore, during the actual installation of the column connector assembly 2, the conical seal 212 can be placed first within the sealing section 122, and then the threaded connection 211... 11 is connected to the connection section 121 by screwing in the thread. When the threaded connection part 211 is tightened, the end face of the threaded connection part 211 presses tightly against the end face of the conical sealing part 212, so that the threaded connection part 211 can push the conical sealing part 212 deeper into the sealing section 122. Due to the obstruction of the inner peripheral edge of the stepped surface 123, the threaded connection part 211 and the inner peripheral edge of the stepped surface 123 squeeze the conical sealing part 212, so that the conical sealing part 212 presses tightly against the inner peripheral edge of the stepped surface 123, thereby achieving a reliable sealing effect.

[0042] In some embodiments, the chromatographic column connector assembly 2 further includes an inner fixing tube 23, a main through hole 2111 is formed in the threaded connection portion 211, and a fixing through hole 2121 is formed in the conical sealing portion 212. The inner diameter of the main through hole 2111 is larger than the inner diameter of the fixing through hole 2121. The inner fixing tube 23 is sequentially inserted into the main through hole 2111 and the fixing through hole 2121 and clamped and fixed at the fixing through hole 2121.

[0043] Specifically, such as Figure 2 As shown, the column connector assembly 2 also includes an inner fixing tube 23, which is used to fix the chromatographic column 22, such as... Figure 9 and Figure 11As shown, the interior of the threaded connection 211 is hollow to form a main through hole 2111, and the interior of the conical sealing part 212 is also hollow to form a fixed through hole 2121. The main through hole 2111 extends through the axial direction of the threaded connection 211, and the fixed through hole 2121 extends through the axial direction of the conical sealing part 212, so that the main through hole 2111 and the fixed through hole 2121 are connected. Furthermore, the inner diameter of the main through hole 2111 is larger than the inner diameter of the fixed through hole 2121. Therefore, the inner fixed tube 23 can pass through the main through hole 2111 to the fixed through hole 2121. The internal fixation tube 23 can extend to the outside through the fixing through hole 2121. The internal fixation tube 23 is sequentially inserted through the main through hole 2111 and the fixing through hole 2121. The inner peripheral wall of the fixing through hole 2121 can tightly press against the outer peripheral wall of the internal fixation tube 23, clamping and fixing the internal fixation tube 23 at the fixing through hole 2121. This achieves fixation of the internal fixation tube 23, preventing it from shifting or shaking, and preventing gaps from forming between the outer peripheral wall of the internal fixation tube 23 and the inner peripheral wall of the fixing through hole 2121, which could lead to liquid leakage during filling. The chromatographic column 22 is inserted through the internal fixation tube 23. When the conical sealing part 212 tightly presses against the inner peripheral edge of the stepped surface 123, the inner peripheral wall of the conical sealing part 212 presses against the internal fixation tube 23, causing the internal fixation tube 23 to deform and press against the chromatographic column 22, thus stably fixing the chromatographic column 22 within the internal fixation tube 23.

[0044] In some embodiments, such as Figure 9 and Figure 11 As shown, the fixed through hole 2121 includes a guide hole section 21211 and a fixed hole section 21212 connected along the axial direction. The guide hole section 21211 is connected between the fixed hole section 21212 and the main through hole 2111. The guide hole section 21211 and the fixed hole section 21212 are connected. The guide hole section 21211 is used to guide the internal fixation tube 23 so that the internal fixation tube 23 can smoothly enter the fixed hole section 21212. The fixed hole section 21212 is used to clamp and fix the internal fixation tube 23.

[0045] Among them, such as Figure 9 and Figure 10 As shown, the inner diameter of the guide hole section 21211 is designed to gradually decrease along the direction close to the fixing hole section 21212. The inner diameter of the fixing hole section 21212 can be set to remain constant, and the inner diameter of the fixing hole section 21212 can be set to be the same as the minimum inner diameter of the guide hole section 21211. The inner diameter of the fixing hole section 21212 can be set to be slightly smaller than the outer diameter of the inner fixing tube 23. In this way, the inner fixing tube 23 can first pass smoothly through the main through hole 2111, and then be guided by the guide hole section 21211 to extend into the fixing hole section 21212 and be clamped and fixed at the fixing hole section 21212.

[0046] It should be noted that, for example Figure 9 and Figure 11 As shown, since the inner diameter of the main through hole 2111 and the inner diameter of the guide hole section 21211 are both larger than the outer diameter of the inner fixing tube 23, a certain gap is formed between the inner peripheral wall of the main through hole 2111 and the inner peripheral wall of the guide hole section 21211 and the outer peripheral wall of the inner fixing tube 23. This gap can accommodate the structural component used to pre-tighten the inner fixing tube 23, that is, the structural component can extend into this gap to push the inner fixing tube 23 to be clamped and fixed more stably at the fixing hole section 21212.

[0047] In some embodiments, a filling cavity 13 is formed in the filling module 1, and the packing port 11 and the chromatographic column interface 12 are connected through the filling cavity 13.

[0048] Specifically, such as Figure 6 and Figure 8 As shown, the filling module 1 has an internal cavity, which is the filling cavity 13, as follows. Figure 2 As shown, the packing port 11 is open to the outside and communicates with the packing cavity 13. In this way, the packing material can be added into the packing cavity 13 through the packing port 11. At the same time, the column interface 12 is communicated with the packing cavity 13, so that the packing material can enter the column interface 12 and fill the column 22.

[0049] In some embodiments, the column interface 12 can be configured as one or more, that is, the column interface 12 can be configured as one, two, three, four or even more, so that one or more columns 22 can be filled simultaneously through one or more column interfaces 12 to meet different needs.

[0050] Furthermore, there are at least two column interfaces 12, and each of the at least two column interfaces 12 is connected to the packing cavity 13. There are at least two column connector assemblies 2, and they are installed in a one-to-one correspondence with the at least two column interfaces 12.

[0051] In other words, the column interface 12 can be configured with two, three, or even more, and each column interface 12 can be connected to the packing cavity 13, so that the packing material in the packing cavity 13 can flow to each column interface 12. The column connector assembly 2 can also be configured with two, three, or even more, and the number of column connector assemblies 2 should be the same as the number of column interfaces 12, so that each column connector assembly 2 can be installed in the corresponding column interface 12. In this way, the packing material flowing to each column interface 12 can fill the corresponding column 22, thereby realizing the synchronous filling of multiple columns 22, greatly improving the packing efficiency of the column 22, meeting the needs of batch preparation, and improving the preparation efficiency.

[0052] In a specific embodiment, such as Figure 3 As shown, there are three column interfaces 12 and three column connector assemblies 2. The filling cavity 13 can be located in the middle area of ​​the filling module 1. The three column interfaces 12 are respectively connected to the filling cavity 13. The three column connector assemblies 2 are installed one-to-one with the three column interfaces 12, so that the three columns 22 can be filled synchronously.

[0053] It should be noted that the number of column interfaces 12 and column connector assemblies 2 is not limited to those described in this embodiment, and can be flexibly set according to actual needs.

[0054] In some embodiments, the filling module 1 is constructed as a cubic block structure and has multiple structural surfaces 14. The filling port 11 and the chromatographic column interface 12 are respectively located on two adjacent structural surfaces 14, and at least two structural surfaces 14 are respectively provided with a chromatographic column interface 12.

[0055] Specifically, the cubic structure can be a regular cubic block or an irregular cubic block, such as a square block, a rectangular block, or other multi-faceted block structures. The filling module 1 has multiple structural faces 14. The filling port 11 and the chromatographic column interface 12 can be respectively located on two adjacent structural faces 14, so that the filling material can be filled into the filling cavity 13 on one structural face 14, and the chromatographic column 22 can be filled on another structural face 14, which is quick and efficient. Furthermore, at least two structural faces 14 each have a chromatographic column interface 12, meaning that chromatographic column interfaces 12 can be set on two, three, or more structural faces 14 to achieve simultaneous filling of multiple chromatographic columns 22.

[0056] In a specific embodiment, such as Figure 3 and Figure 4 As shown, the filling module 1 is constructed as a cube. The filling module 1 has six structural surfaces 14. The filling port 11 and the chromatographic column interface 12 are respectively located on two adjacent structural surfaces 14, and three chromatographic column interfaces 12 are provided. Each of the three structural surfaces 14 has one chromatographic column interface 12.

[0057] In some embodiments, the capillary column packing apparatus 100 further includes a magnetic stirrer, wherein the packing chamber 13 is filled with a magnetic stir bar, and the magnetic stirrer is used to drive the magnetic stir bar to stir within the packing chamber 13.

[0058] Specifically, when the magnetic stirrer is powered on, it generates a rotating magnetic field that interacts with the magnet in the magnetic stir bar, driving the stir bar to move in a circular motion and achieving a stirring effect. In the actual process of filling the chromatographic column 22 using the capillary column packing apparatus 100, the packing port 11 can be opened first, and the packing material added to the packing cavity 13. Then, the magnetic stir bar can be placed inside the packing cavity 13, and the packing port 11 can be sealed to prevent liquid leakage. High-pressure liquid medium is then introduced, and the magnetic stirrer is powered on to start stirring. This allows the magnetic stirrer to drive the magnetic stir bar to stir the packing material and high-pressure liquid medium within the packing cavity 13, ensuring uniform mixing and guaranteeing that the packing material is packed into the chromatographic column 22 at a stable concentration.

[0059] It should be noted that the mixing effect between the packing material and the high-pressure liquid medium can be optimized by adjusting the stirring speed of the magnetic stirrer.

[0060] In some embodiments, the capillary column synchronous packing apparatus 100 further includes a constant pressure pump 3, which is connected to a pressure supply interface 15. The constant pressure pump 3 provides pressure to the packing module 1 through the pressure supply interface 15 so that the packing material at the packing port 11 moves toward the column interface 12.

[0061] Specifically, the constant pressure pump 3 can be a gas constant pressure pump or a liquid constant pressure pump, that is, the constant pressure pump 3 can pump high-pressure liquid or high-pressure gas into the packing chamber 13 to achieve the packing of the chromatographic column 22. Preferably, the constant pressure pump 3 is set as a liquid constant pressure pump, and the pressure supply port 15 is used to allow the liquid medium to flow into the packing module 1, and the pressure is transmitted through the liquid medium to push the packing material to fill the chromatographic column 22. Figure 1 As shown, the pressure supply port 15 is connected to the constant pressure pump 3. In this way, the constant pressure pump 3 can provide stable power to drive the liquid medium to enter the packing chamber 13 through the pressure supply port 15. In the packing chamber 13, the liquid medium mixes with the packing material, and the pressure transmitted by the liquid medium causes the packing material to move towards the column interface 12, so that the packing material is uniformly filled in the column 22.

[0062] In practical design, such as Figure 2 As shown, after filling the filling cavity 13 with packing material through the packing port 11, the sealing member 5 can be used to seal the packing port 11, thereby achieving a seal and preventing leakage of packing material and liquid medium. The sealing member 5 can be a sealing nut or other structural component, such as... Figure 8 As shown, a sealing gasket 6 can also be provided between the filling port 11 and the sealing member 5 to further improve the sealing performance.

[0063] In some embodiments, the constant pressure pump 3 is connected to the pressure supply interface 15 via the pressure supply pipe 4. The pressure supply pipe 4 is provided with a connecting joint 41, which is threadedly connected to the pressure supply interface 15. The pressure supply interface 15 is provided with a sealing ring that seals against the end face of the connecting joint 41.

[0064] Specifically, the constant pressure pump 3 can be a gas constant pressure pump or a liquid constant pressure pump, that is, the constant pressure pump 3 can pump high-pressure liquid or high-pressure gas into the packing chamber 13 to achieve the packing of the chromatographic column 22, such as... Figure 1 and Figure 2 As shown, the constant pressure pump 3 is configured as a liquid constant pressure pump, and the explanation will be based on the liquid constant pressure pump. The constant pressure pump 3 is connected to the pressure supply interface 15 through the pressure supply pipe 4. The pressure supply pipe 4 is provided with a connecting joint 41. An internal thread can be provided on the inner peripheral wall of the pressure supply interface 15, and an external thread that matches the internal thread can be provided on the outer peripheral wall of the connecting joint 41. The connecting joint 41 and the pressure supply interface 15 are threadedly connected by the mutual engagement of the internal thread and the external thread, thereby achieving a tight connection between the pressure supply pipe 4 and the pressure supply interface 15. Thus, the constant pressure pump 3 can pump high-pressure liquid medium into the packing cavity 13 through the pressure supply pipe 4, so that the liquid medium mixes with the packing material, and the high-pressure liquid medium pushes the packing material to fill the chromatographic column 22.

[0065] Furthermore, a sealing ring can be provided in the pressure supply interface 15 to seal against the end face of the connecting joint 41, that is, one side of the sealing ring is tightly pressed against the end face of the connecting joint 41 to prevent gaps from forming at the connection between the pressure supply interface 15 and the connecting joint 41, which would lead to leakage of liquid medium, thereby further improving the sealing performance of the capillary chromatography column synchronous packing instrument 100.

[0066] Therefore, the capillary column synchronous packing device 100 of this application is free from dependence on liquid chromatograph and can operate independently with only a constant pressure pump 3. At the same time, it can develop a modular and low-cost consumable system to reduce the cost of packing accessories. Moreover, it only requires a constant pressure pump 3, a column connector assembly 2 and a packing module 1, without the need for an HPLC instrument, making it more widely applicable and improving the deployment feasibility of small and medium-sized laboratories. In addition, all interfaces can adopt universal sizes to adapt to various connectors, making assembly simple.

[0067] In other embodiments, the fixing joint 21 is made of a metal material, such as stainless steel, and the inner fixing tube 23 can be constructed as a PEEK tube. In practical design, the fixing joint 21 can adopt a standardized design to enable standardized production, thus broadening its applicability and making manufacturing more convenient.

[0068] In other embodiments, such as Figure 12 and Figure 13As shown, the packing port 11 can be integrated with the column interface 12, meaning the packing port 11 is also configured as the column interface 12. In practical designs, such as... Figure 13 As shown, a connecting section 121 and a sealing section 122 can be provided in the sealing member 5, so that the chromatographic column connector assembly 2 can be inserted into the sealing member 5.

[0069] The specific packing operation procedure of the capillary column synchronous packing instrument 100 of this application is as follows: S1. The capillary is burned with the outer flame of an alcohol lamp until the polyimide surface is charred and falls off. The surface of the capillary is gently wiped with cotton paper soaked in 75% ethanol to remove the charred surface. Then the capillary with the polyimide coating removed is placed into a laser needle drawing instrument to draw it into a capillary chromatographic column 22 with good spray. S2, filling module 1, fixing connector 21 and all accessories of filling module 1 are placed in a beaker, and an organic solvent (methanol, acetonitrile, isopropanol organic solvent can be used) is added for ultrasonic cleaning. After ultrasonic rinsing, the beaker is dried. 10mg of filler powder is added to the filling port 11 of filling module 1, then a magnetic stir bar is added, and then two sealing gaskets 6 are added to seal the sealing part 5 in the filling port 11. S3. Carefully insert the drawn capillary column 22 into the fixed connector 21. Note that the tail end of the capillary column 22 extends 3mm beyond the tip of the fixed connector 21. Then, insert the fixed connector 21 into the column interface 12. S4. Power on the constant pressure pump 3 and turn on the power switch. Connect an acetonitrile pipe to the liquid inlet and a pre-column to the liquid outlet. Tighten the drain valve knob clockwise. Then press the PURGE button on the control panel. After liquid continues to flow steadily from the pre-column outlet, press the STOP button to stop the air bubble removal. S5. Connect the pressure supply interface 15 of the filling module 1 to the other end of the pre-column, set the magnetic stirrer to 600 rpm, and then press the pump button on the control panel of the constant pressure pump 3 to start filling. Observe whether the packing material fills the capillary column 22 completely.

[0070] In the description of this specification, the references to terms such as "one embodiment," "some embodiments," "illustrative embodiment," "example," "specific example," or "some examples," etc., indicate that a specific feature, structure, material, or characteristic described in connection with that embodiment or example is included in at least one embodiment or example of the present invention. In this specification, the illustrative expressions of the above terms do not necessarily refer to the same embodiment or example. Furthermore, the specific features, structures, materials, or characteristics described may be combined in any suitable manner in one or more embodiments or examples.

[0071] Although embodiments of the present invention have been shown and described, those skilled in the art will understand that various changes, modifications, substitutions and alterations can be made to these embodiments without departing from the principles and spirit of the present invention, the scope of which is defined by the claims and their equivalents.

Claims

1. A capillary chromatographic column simultaneous packing apparatus characterized by comprising: include: The filling module (1) and the column connector assembly (2) are provided. The filling module (1) is provided with a packing port (11), a pressure supply port (15) and a column interface (12). The pressure supply port (15), the packing port (11) and the column interface (12) are all connected. The column connector assembly (2) includes a fixed connector (21) and a column (22). The fixed connector (21) is inserted into the column interface (12) and the column (22) passes through the fixed connector (21). The chromatographic column interface (12) includes a connecting section (121) and a sealing section (122). The inner diameter of the connecting section (121) is larger than the inner diameter of the sealing section (122) to form a stepped surface (123) at the connection between the connecting section (121) and the sealing section (122). The fixed connector (21) includes a threaded connection part (211) and a conical sealing part (212). The threaded connection part (211) is threadedly connected to the connecting section (121). At least a portion of the conical sealing part (212) extends into the sealing section (122) and the conical sealing part (212) presses against the inner periphery of the stepped surface (123).

2. The capillary column slurry filler of claim 1, wherein, The stepped surface (123) is constructed as an inner conical surface. The inner diameter of the inner conical surface is set to gradually decrease from the end connected to the connecting section (121) to the end connected to the sealing section (122). The outer peripheral wall of the conical sealing part (212) is formed with an outer conical surface (2122). The outer conical surface (2122) is sealed and pressed against the end of the inner conical surface connected to the sealing section (122).

3. The capillary column slurry filler of claim 2, wherein, The angle between the outer conical surface (2122) and the fixed joint (21) is smaller than the angle between the inner conical surface and the axial direction of the chromatographic column interface (12).

4. The capillary column slurry filler of claim 1, wherein, The threaded connection (211) and the conical sealing part (212) are integrally formed parts; Alternatively, the threaded connection (211) and the conical sealing part (212) are separate parts, and the end face of the threaded connection (211) presses against the end face of the conical sealing part (212).

5. The capillary column slurry filler of claim 1, wherein, The chromatographic column connector assembly (2) also includes an inner fixing tube (23). A main through hole (2111) is formed in the threaded connection part (211), and a fixing through hole (2121) is formed in the conical sealing part (212). The inner diameter of the main through hole (2111) is larger than the inner diameter of the fixing through hole (2121). The inner fixing tube (23) is sequentially inserted through the main through hole (2111) and the fixing through hole (2121) and clamped and fixed at the fixing through hole (2121).

6. The capillary column slurry filler of claim 5, wherein, The fixed through hole (2121) includes a guide hole section (21211) and a fixed hole section (21212) connected along the axial direction. The guide hole section (21211) is connected between the fixed hole section (21212) and the main through hole (2111). The inner diameter of the guide hole section (21211) is gradually reduced along the direction close to the fixed hole section (21212). The inner fixed tube (23) is clamped and fixed at the fixed hole section (21212).

7. The capillary column packing apparatus according to claim 1, characterized in that, The filling module (1) has a filling cavity (13) formed therein, and the packing port (11) and the chromatographic column interface (12) are connected through the filling cavity (13); Among them, there are at least two chromatographic column interfaces (12), and at least two chromatographic column interfaces (12) are respectively connected to the filling cavity (13). There are at least two chromatographic column connector assemblies (2) and they are installed one-to-one with at least two chromatographic column interfaces (12).

8. The capillary column slurry filler of claim 7, wherein, The filling module (1) is constructed as a cubic block structure and has multiple structural surfaces (14). The filling port (11) and the chromatographic column interface (12) are respectively located on two adjacent structural surfaces (14), and at least two structural surfaces (14) are respectively provided with a chromatographic column interface (12).

9. The capillary column packing apparatus according to claim 7, characterized in that, It also includes a magnetic stirrer, wherein the filling cavity (13) is filled with a magnetic stir bar, and the magnetic stirrer is used to drive the magnetic stir bar to stir in the filling cavity (13).

10. The capillary column packing apparatus according to claim 1, characterized in that, It also includes a constant pressure pump (3), which is connected to the pressure supply interface (15). The constant pressure pump (3) provides pressure to the packing module (1) through the pressure supply interface (15) so that the packing material at the packing port (11) moves toward the column interface (12).

11. The capillary column slurry filler of claim 10, wherein, The constant pressure pump (3) is connected to the pressure supply interface (15) through the pressure supply pipe (4). The pressure supply pipe (4) is provided with a connecting joint (41). The connecting joint (41) is threadedly connected to the pressure supply interface (15), and the pressure supply interface (15) is provided with a sealing ring that seals against the end face of the connecting joint (41).

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