CN113374950A - High pressure resistant liquid chromatography connects and realizes zero dead volume's fluidic connected system - Google Patents

Abstract

The invention discloses a high pressure resistant liquid chromatography joint and a fluid type connecting system for realizing zero dead volume; a high pressure resistant liquid chromatography joint comprising: the assembling nut comprises an external thread and a fastening end face, and an axial hole I penetrates through the assembling nut; the hoop comprises a compression end face and an extension section, the compression end face is abutted against the compression end face, and a second axial hole for allowing the pk tube to pass through penetrates through the hoop; the peek tube comprises a tube body and a bearing end, wherein a third axial hole for the capillary tube to penetrate through penetrates through the inside of the peek tube, the tube body is embedded into the second axial hole, and one end of the tube body extends into the first axial hole. The high pressure resistant liquid chromatography joint in the technical scheme has strong adaptability and can be adapted to the 1/16' joint with 10-32 threads on the market.

Description

High pressure resistant liquid chromatography connects and realizes zero dead volume's fluidic connected system

Technical Field

The invention relates to the technical field of chromatography, in particular to a high pressure resistant liquid chromatography joint and a fluid type connecting system for realizing zero dead volume.

Background

High Performance Liquid Chromatography (HPLC) is a high-efficiency and rapid analysis and separation technology developed in the seventies of the 20 th century, and is an important means of modern biochemical analysis. The basic separation principle of chromatography is: when each component dissolved in the mobile phase passes through the stationary phase, the components are retained in the stationary phase for different time periods due to different sizes and strengths of the components which are acted (adsorbed, distributed, excluded and affinity) with the stationary phase, and then flow out of the stationary phase successively.

HPLC has been developed based on classical liquid chromatography, using a column chromatography separation technique with a liquid as the mobile phase and a fine-grained high performance stationary phase. The separation mechanism is the same as that of the conventional column chromatography, but the filler is finer and needs to be pushed by a high-pressure pump, the column efficiency is high, and the analysis speed is high.

The high performance liquid chromatography uses a high pressure infusion pump, a full porous particle packed column and a high sensitivity detector to realize the high speed, high efficiency and high sensitivity separation and measurement of the sample.

The application range of the high performance liquid chromatography is very wide, and the high performance liquid chromatography is widely used for research in the fields of analytical chemistry, biochemistry, chemical biology, pharmacy and the like. . HPLC is widely used in the field of chemical analysis because of its characteristics of high separation efficiency, high analysis speed, good detection sensitivity, ability to analyze and separate thermally unstable physiologically active substances having a high boiling point and being unable to vaporize. High pressure HPLC systems require high pressure resistant joints to ensure the tightness of the system. In addition, for a liquid phase with a nanoliter flow rate, the dead volume at the joint can seriously affect the peak time and reduce the separation efficiency of the liquid phase, so that a liquid joint with zero dead volume is an indispensable part in nanoliter-level liquid chromatography.

A common high-pressure resistant 1/16' chromatographic joint on the market generally integrates three parts together, and is sealed by the extrusion of a peek pipe at the front end of the joint, and the sealed pipeline made of the peek material is abraded due to the frequent extrusion of the pipeline, so that the joint is damaged.

Disclosure of Invention

The present invention aims to overcome the disadvantages of the prior art and to provide a high pressure resistant liquid chromatography joint and a fluidic connection system that achieves zero dead volume, compared to the prior art

The invention is realized by the following technical scheme:

a high pressure resistant liquid chromatography joint comprising: the assembling nut comprises an external thread and a fastening end face, and an axial hole I penetrates through the assembling nut; the hoop comprises a compression end face and an extension section, the compression end face is abutted against the compression end face, and a second axial hole for allowing the pk tube to pass through penetrates through the hoop; the peek tube comprises a tube body and a bearing end, wherein a third axial hole for the capillary tube to penetrate through penetrates through the inside of the peek tube, the tube body is embedded into the second axial hole, and one end of the tube body extends into the first axial hole.

As a preferable scheme of the high pressure resistant liquid chromatography joint: the assembly nut with the staple bolt is stainless steel.

As a preferable scheme of the high pressure resistant liquid chromatography joint: the diameter of the axial hole III is 360 mu m.

In the technical proposal, the device comprises a base,

a fluidic connection system for achieving zero dead volume, comprising a high pressure tolerant liquid chromatography joint, comprising:

the liquid phase two-way connector is characterized in that two ends of the liquid phase two-way connector are respectively provided with a port, the inner wall of each port is provided with an internal thread, the internal thread is matched and connected with the external thread, the inner side of each port is provided with a reducing port, the section of each reducing port is of a trapezoidal structure, and the inner side of each reducing port is provided with a passage port which communicates the two reducing ports;

the external thread of the assembling nut is screwed with the internal thread;

the extending section of the hoop extends into the channel opening, and the fastening end face of the assembling nut is tightly pressed with the pressing end face of the hoop;

the peek pipe is embedded into the hoop, the bearing ends of the peek pipe extend into the channel opening, and the end faces of the two bearing ends are abutted to form a face sealing structure;

a capillary tube passing through the fitting nut and the peek tube.

The invention is further provided with: the diameter of the port is larger than that of the passage opening, the diameter of one side, close to the passage opening, of the reducing opening is smaller than that of the port, and the diameter of one side, close to the passage opening, of the reducing opening is equal to that of the passage opening.

The invention discloses a high pressure resistant liquid chromatography joint and a fluid type connecting system for realizing zero dead volume, compared with the prior art:

1. according to the high-pressure-resistant liquid chromatography joint, the stainless steel assembly nut, the stainless steel hoop and the peek pipe are combined, the hoop and the peek pipe are tightly pressed by the assembly nut, end face sealing is achieved, and the high-pressure bearing capacity of the joint is greatly improved;

2. the high pressure resistant liquid chromatography joint in the technical scheme has strong adaptability and can be adapted to the existing 1/16' joint with 10-32 threads on the market;

3. according to the technical scheme, the fluid type connecting system for realizing the zero dead volume compresses the hoop and the peek pipes through the assembling nuts, and the end faces of the bearing ends of the two peek pipes compress the end faces in an extruding mode, so that the real zero dead volume is realized, and the liquid phase separation efficiency is improved.

Drawings

FIG. 1 is an isometric view of a high pressure tolerant liquid chromatography joint of the present invention.

Figure 2 is a front view of a high pressure resistant liquid chromatography fitting of the present invention.

Figure 3 is a cross-sectional view of a high pressure resistant liquid chromatography fitting of the present invention.

Figure 4 is a schematic, broken away cross-sectional view of a high pressure tolerant liquid chromatography joint of the present invention.

FIG. 5 is a cross-sectional view of a mounting nut of the high pressure liquid chromatography resistant fitting of the present invention.

Fig. 6 is a cross-sectional view of the hoop of the high pressure resistant liquid chromatography fitting of the present invention.

FIG. 7 is a cross-sectional view of a peek tube of a high pressure tolerant liquid chromatography fitting of the present invention.

FIG. 8 is a schematic structural diagram of a conventional liquid chromatography two-way pipe to which the high pressure resistant liquid chromatography fitting of the present invention is applied.

Fig. 9 is a schematic diagram of the structure of the liquid phase two-way joint of the present invention for a fluid-type connection system that achieves zero dead volume.

Fig. 10 is a schematic diagram of the present invention fluid coupling system to achieve zero dead volume.

Fig. 11 is an enlarged view of the plane a in fig. 10, in order to show the face seal structure.

The corresponding part names indicated by the numbers and letters in the drawings:

wherein: 10. assembling a nut; 10a, external threads; 10b, tightly breaking the end face; 10c, a first axial hole; 10d, a screwing end; 10e, a main body end; 20. hooping; 20a, pressing the end face; 20b, an extension section; 20c, a second axial hole; 20d, pressing blocks; 30. a peek tube; 30a, a tube body; 30b, a bearing end; 30c, a third axial hole; 30b1, end face; 40. a capillary tube; 50. a liquid phase two-way joint; 50a, a port; 50b, internal threads; 50c, a variable diameter opening; 50d, a channel port; 60. a face seal structure; 70. a liquid chromatography two-way line; 70a, port one; 70b, a first variable-diameter opening; 70c, installing a port; 70d, channel port one.

Detailed Description

The technical scheme of the invention is further explained by the specific implementation mode in combination with the attached drawings.

Wherein the showings are for the purpose of illustration only and are shown by way of illustration only and not in actual form, and are not to be construed as limiting the present patent; to better illustrate the embodiments of the present invention, some parts of the drawings may be omitted, enlarged or reduced, and do not represent the size of an actual product; it will be understood by those skilled in the art that certain well-known structures in the drawings and descriptions thereof may be omitted.

The same or similar reference numerals in the drawings of the embodiments of the present invention correspond to the same or similar components; in the description of the present invention, it should be understood that if the terms "upper", "lower", "left", "right", "inner", "outer", etc. are used for indicating the orientation or positional relationship based on the orientation or positional relationship shown in the drawings, it is only for convenience of description and simplification of description, but it is not indicated or implied that the referred device or element must have a specific orientation, be constructed in a specific orientation and be operated, and therefore, the terms describing the positional relationship in the drawings are only used for illustrative purposes and are not to be construed as limitations of the present patent, and the specific meanings of the terms may be understood by those skilled in the art according to specific situations.

Referring to fig. 1-4, a high pressure tolerant liquid chromatography fitting comprises: the assembling nut 10 comprises an external thread 10a and a fastening end face 10b, and an axial hole 10c penetrates through the assembling nut 10; the hoop 20 comprises a pressing end face 20a and an extension section 20b, the breaking end face 10b is abutted against the pressing end face 20a, and a second axial hole 20c for the peek pipe 30 to pass through penetrates through the hoop 20; the Peek tube 30 includes a tube body 30a and a bearing end 30b, an axial hole three 30c for the capillary tube 40 to pass through is penetrated through the inside of the Peek tube 30, the tube body 30a is embedded in the axial hole two 20c, and one end of the tube body extends into the axial hole one 10 c.

As shown in detail in fig. 5, the assembly nut 10 further includes a screwing end 10d and a main body end 10e disposed at one side of the screwing end 10d, the screwing end 10d is used for screwing the whole assembly nut 10 and a socket one 70a of the two-way liquid chromatography conduit 70 by using a wrench (including an electric wrench or a manual wrench), the main body end 10e is cylindrical, the external thread 10a is disposed on an outer wall of the main body end 10e, and the fastening end face 10b is disposed at one side of the main body end 10e away from the screwing end 10 d; it is noted that the tightening end 10d is preferably a regular hexagon head, and the axial hole one 10c penetrates through the inside of the body end 10e and the tightening end 10 d; furthermore, the fitting nut 10 is one-piece;

as shown in detail in fig. 6, the anchor ear 20 further includes a pressing block 20d, the extension section 20b is disposed on one side of the pressing block 20d, the pressing block 20d has a disc-shaped structure, the diameter of the pressing block 20d is the same as that of the main body end 10e, the pressing end surface 20a is located on one side of the pressing block 20d away from the extension section 20b, the extension section 20b is cylindrical, and the second axial hole 20c penetrates through the pressing block 20d and the extension section 20 b; notably, the diameters of the first axial hole 10c and the second axial hole 20c are the same, and the diameter of the first axial hole 10c is larger than that of the third axial hole 30 c; in addition, the hoop 20 is integrated;

referring in detail to fig. 7, the bearing end 30b of the peek tube 30 is cylindrical, the diameter of the bearing end 30b is the same as the diameter of the extension 20b, the peek tube 30 is made of peek material, and the peek tube 30 is one-piece;

in summary, referring to fig. 8 in detail, fig. 8 is a schematic structural diagram of the high pressure resistant liquid chromatography joint applied to a conventional liquid chromatography two-way pipeline, two ends of the liquid chromatography two-way pipeline 70 are respectively provided with a port one 70a, the inner wall of the port one 70a is provided with an internal thread one, the internal thread one is connected with the external thread 10a in a matching manner, the inner side of the port one 70a is provided with a reducing port one 70b, the section of the reducing port one 70b is in a trapezoidal structure, the inner side of the first reducing port 70b is provided with a mounting port 70c, a first channel port 70d is arranged between the two mounting ports 70c, the first channel port 70d can be used for the capillary tube 40 to pass through, the diameter of the port one 70a is larger than that of the mounting port 70c, the diameter of the side of the reducing port one 70b close to the port one 70a is smaller than that of the port one 70a, the diameter of the side of the reducing port one 70b away from the port one 70a is equal to the diameter of the mounting port 70 c. The installation principle of the high pressure resistant liquid chromatography joint of the technical scheme is as follows: firstly, the peek tube 30 is embedded into the hoop 20, the bearing end 30b of the peek tube 30 is located outside the extending section 20b and the bearing end 30b is abutted against the extending section 20b, then the hoop 20 is inserted into the installation port 70c of the liquid chromatography pipeline 70, then the hoop 20 is preliminarily pressed by the assembly nut 10, the capillary tube 40 sequentially passes through the assembly nut 10 and the peek30 embedded inside the hoop 20, then the external thread 10a of the assembly nut 10 is screwed with the internal thread of the liquid chromatography pipeline 70, with the continuous screwing of the assembly nut 10, the broken end face 10b of the assembly nut 10 is continuously pressed towards the pressing end face 20a of the hoop 20, so that the bearing end 30b of the peek tube 30 and the side wall of the installation port 70c close to the first passage port 70d are tightly pressed, that is continuously screwed into the liquid chromatography pipeline 70 by the assembly nut 10, the tight end face 10b of the assembling nut 10 and the compression end face 20a of the hoop 20 are compressed to realize sealing, the assembling nut 10 and the hoop 20 are two independent accessories, and the assembling nut 10 and the hoop 20 realize extrusion compression by virtue of the assembling nut 10, so that the sealing effect of the assembling nut 10, the hoop 20, the peek pipe 30 and the liquid chromatography two-way pipeline 70 is realized; it should be noted that, for convenience of understanding, the liquid chromatography two-way pipe 70 is described in terms of structure, the liquid chromatography two-way pipe 70 is the prior art, and a person skilled in the art can select the liquid chromatography two-way pipe according to actual needs.

As one of the preferred embodiments of the high pressure resistant liquid chromatography joint: the assembly nut 10 and the hoop 20 are made of stainless steel. According to the technical scheme, the assembling nut 10 and the hoop 20 which are made of stainless steel materials are adopted, the bearing end 30b of the peek pipe 30 is matched with the tight contact of the mounting port 70c, namely the head of the peek pipe 30 is sealed, and the high-pressure bearing capacity of the joint is improved.

As another preferred embodiment of the high pressure resistant liquid chromatography joint: the diameter of the axial hole three 30c is 360 μm. The technical scheme can be used for pipelines made of different materials such as quartz capillary tubes, metal tubes, peek tubes and the like with the outer diameter of 360 mu m to pass through.

In addition, as a high pressure resistant liquid chromatography joint, it should be noted that the tube 30a is inserted into the second axial hole 20c and one end of the tube extends into the first axial hole 10c, that is, the outer diameter of the tube 30a is the same as the diameter of the first axial hole 10c, and at the same time, one end of the tube 30a extends into the first axial hole 10c, that is, one end of the tube 30a extends into the assembly nut 10a, so that the assembly nut 10, the hoop 20 and the peek tube are conveniently installed, and the offset is prevented.

Referring to fig. 1-11, a fluid coupling system for achieving zero dead volume, including a high pressure tolerant liquid chromatography fitting, includes: the liquid phase two-way connector 50 is provided with ports 50a at two ends, an inner wall of each port 50a is provided with an inner thread 50b, each inner thread 50b is matched and connected with the corresponding outer thread 10a, a reducing port 50c is arranged on the inner side of each port 50a, the section of each reducing port 50c is of a trapezoidal structure, a passage port 50d is arranged on the inner side of each reducing port 50c, and the passage ports 50d are communicated with the two reducing ports 50 c; the assembling nut 10 is characterized in that an external thread 10a and an internal thread 50b of the assembling nut 10 are screwed; the anchor ear 20, the extension section 20b of the anchor ear 20 extends into the channel opening 50d, and the fastening end face 10b of the assembly nut 10 is pressed against the pressing end face 20a of the anchor ear 20; the peek pipe 30 is embedded in the hoop 20, the bearing end 30b of the peek pipe 30 extends into the passage opening 50d, and the end surfaces 30b1 of the two bearing ends 30b are abutted to form a surface sealing structure 60; a capillary tube 40, said capillary tube 40 passing through the fitting nut 10 and the peek tube 30. It is noted here that, with regard to the fluid connection system for achieving zero dead volume, as shown in detail in fig. 10, the capillary tube 40 passes through the left fitting nut 10, the left peek tube 30, the right peek tube 30 and the right fitting nut 10 in this order from left to right, that is, the fluid connection system for achieving zero dead volume is achieved by the cooperation between the liquid two-way joint 50, the two high pressure resistant liquid chromatography joints and the capillary tube.

As a preferred embodiment of the fluidic connection system to achieve zero dead volume: the diameter of the port 50a is larger than that of the passage port 50d, the diameter of the side of the reducing port 50c close to the port 50a is smaller than that of the port 50a, and the diameter of the side of the reducing port 50c close to the passage port 50d is equal to that of the passage port 50 d.

Referring to fig. 10 and 11 in detail, firstly, the peek tube 30 is inserted into the hoop 20, the carrying end 30b of the peek tube 30 contacts the extension section 20b of the hoop 20, then the two hoops 20 are respectively inserted into the two ports 50a of the liquid phase two-way joint 50 and the carrying end 30b is inserted into the passage port 50d, then the two assembly nuts 10 are respectively screwed into the two ports 50a to achieve preliminary compression, the capillary tube 40 sequentially passes through the right assembly nut, the right peek tube, the left peek tube and the left assembly nut from right to left to achieve pre-fixing of the capillary tube 40, then the assembly nuts 10 are continuously screwed, the broken end face 10b of the assembly nut 10 presses the hoop 20, so that the end faces 30b1 of the carrying ends 30b of the two peek tubes 30 are pressed, and the face sealing structure 60 is formed between the two end faces 30b1, thereby realizing real zero dead volume and improving the liquid phase separation efficiency.

The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be able to cover the technical scope of the present invention and the equivalent alternatives or modifications according to the technical solution and the inventive concept of the present invention within the technical scope of the present invention.

It is noted that, herein, relational terms such as first and second, and the like may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus. Without further limitation, an element defined by the phrase "comprising an … …" does not exclude the presence of other identical elements in a process, method, article, or apparatus that comprises the element.

Claims (5)

1. High pressure resistant liquid chromatography connects, its characterized in that includes:

the assembling nut (10) comprises an external thread (10a) and a fastening end face (10b), and an axial hole I (10c) penetrates through the assembling nut (10);

the hoop (20) comprises a pressing end face (20a) and an extending section (20b), the breaking end face (10b) is abutted to the pressing end face (20a), and a second axial hole (20c) for a peek pipe (30) to penetrate through is formed in the hoop (20);

the Peek pipe (30) comprises a pipe body (30a) and a bearing end (30b), an axial hole III (30c) for a capillary (40) to penetrate through is formed in the Peek pipe (30), the pipe body (30a) is embedded in the axial hole II (20c), and one end of the pipe body extends into the axial hole I (10 c).

2. The high pressure resistant liquid chromatography joint of claim 1, wherein: the assembling nut (10) and the hoop (20) are made of stainless steel.

3. The high pressure resistant liquid chromatography joint of claim 1, wherein: the diameter of the axial hole three (30c) is 360 μm.

4. A fluidic coupling system for achieving zero dead volume comprising a high pressure tolerant liquid chromatography joint according to any of claims 1-3, comprising:

the liquid phase two-way connector (50) is provided with ports (50a) at two ends, an internal thread (50b) is arranged on the inner wall of each port (50a), the internal thread (50b) is matched and connected with the external thread (10a), a reducing port (50c) is arranged on the inner side of each port (50a), the section of each reducing port (50c) is of a trapezoidal structure, a passage port (50d) is arranged on the inner side of each reducing port (50c), and the passage ports (50d) are communicated with the two reducing ports (50 c);

the assembling nut (10), the external thread (10a) of the assembling nut (10) is screwed with the internal thread (50 b);

the anchor ear (20), an extension section (20b) of the anchor ear (20) extends into the channel opening (50d), and a fastening end face (10b) of the assembling nut (10) is pressed with a pressing end face (20a) of the anchor ear (20);

the peek pipe (30), the peek pipe (30) is embedded into the hoop (20), the bearing ends (30b) of the peek pipe (30) extend into the channel opening (50d), and the end faces (30b1) of the two bearing ends (30b) are abutted to form a face sealing structure (60);

a capillary tube (40), the capillary tube (40) passing through the fitting nut (10) and the peek tube (30).

5. The fluidic coupling system of claim 4, wherein: the diameter of the port (50a) is larger than that of the passage opening (50d), the diameter of the side of the reducing opening (50c) close to the port (50a) is smaller than that of the port (50a), and the diameter of the side of the reducing opening (50c) close to the passage opening (50d) is equal to that of the passage opening (50 d).

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