CN211318328U

CN211318328U - Sample introduction chromatographic bottle for liquid chromatograph

Info

Publication number: CN211318328U
Application number: CN201922447654.XU
Authority: CN
Inventors: 赵芳芳
Original assignee: Chengdu Davidsot Biotechnology Co ltd
Current assignee: Chengdu Davidsot Biotechnology Co ltd
Priority date: 2019-12-30
Filing date: 2019-12-30
Publication date: 2020-08-21
Anticipated expiration: 2029-12-30

Abstract

The utility model relates to a liquid chromatograph is with advancing kind chromatographic bottle, including bottle post, nut, column joint, seal cover, packing ring and pressure cap, bottle post lower extreme coupling nut and column joint, bottle post upper end is by seal cover, packing ring and pressure cap formation sealing joint, sets up the sieve between sealing joint and the bottle post upper end, be used for filling the stationary phase granule in the bottle post, the bottle post inner wall evenly is provided with a plurality of little spines, little spine size is unanimous with stationary phase granule size for little spine pierces in the packing post that the stationary phase granule formed, and this scheme can eliminate basically and is close to the pipe wall position and produces the channelling effect, reduces the liquid phase velocity of flow, thereby improves the analytical accuracy.

Description

Sample introduction chromatographic bottle for liquid chromatograph

Technical Field

The utility model relates to a liquid chromatograph field, concretely relates to liquid chromatograph is with advancing kind chromatographic bottle.

Background

The chromatographic column consists of column tube, pressing cap, clamping sleeve, sieve plate, joint, screw, etc. The column tube is made of stainless steel, when the pressure is not higher than 70 kg/cm2, thick-wall glass or quartz tube can be used, and the inner wall of the tube is required to have high smoothness. In order to improve the column effect and reduce the tube wall effect, the inner wall of the stainless steel column is polished. Fluoroplastics are also coated on the inner wall of the stainless steel column to improve the smoothness of the inner wall, and the effect is the same as that of polishing. Also, use of fused silica or glass liners for thin tubing strings. Sieve plates are arranged in column joints at two ends of the chromatographic column, are sintered stainless steel or titanium alloy and have the aperture of 0.2-20 mu m (5 to 10 μm), depending on the filler particle size, in order to prevent leakage of the filler. The chromatographic column can be divided into an analytical type and a preparative type according to the application, and the size specifications are also different: a conventional analytical column (a constant column) with an inner diameter of 2-5 mm (4.6 mm is commonly used, 4mm and 5mm exist in China) and a column length of 10-30 cm; secondly, narrow-diameter columns (also called thin-diameter columns and semi-microcolumns) with the inner diameter of 1-2 mm and the length of 10-20 cm; thirdly, the inner diameter of the capillary column (also called microcolumn) is 0.2-0.5 mm; preparing a column in half, wherein the inner diameter is more than 5 mm; preparing a column in a laboratory, wherein the inner diameter is 20-40 mm, and the column length is 10-30 cm; sixthly, the inner diameter of the production preparation column can reach dozens of centimeters. The internal diameter of the column is generally determined based on the length of the column, the particle size of the packing and the reduced flow rate in order to avoid wall effects. The column efficiency is influenced by factors inside and outside the column, and in order to achieve the optimal efficiency of the chromatographic column, the dead volume is small except for the column, and the dead volume is from the sample inlet of the sample injector to the space of the detector flow cell which is not occupied by the stationary phase. It includes 4 parts of sample injector to chromatographic column pipeline volume, stationary phase particle gap (occupied by mobile phase, Vm) in the column, column outlet pipeline volume, detector flow cell volume. Only Vm participates in the chromatographic equilibrium process, and the other 3 parts only play a role in peak expansion. To prevent peak spreading, the volume of these 3 portions should be minimized. Reasonable column structure (dead volume outside the packed bed is reduced as much as possible) and packing technique are also needed. Even with the best packing technique, the packing conditions are always different at the central part of the column and along the wall of the tube, the part close to the tube wall is looser, channeling is easy to generate, the flow velocity is high, the flow shape of the flushing agent is influenced, the spectral band is widened, and the tube wall effect is realized. This wall region is approximately 30 particle size thicknesses measured inward from the wall. In a typical liquid chromatography system, the effect of the out-of-column effect on the column effect is much greater than the tube wall effect.

SUMMERY OF THE UTILITY MODEL

An object of the utility model is to overcome prior art's not enough, provide a liquid chromatograph is with advancing kind chromatographic flask, can eliminate basically and be close to the pipe wall position and produce the channeling effect, reduce the liquid phase velocity of flow to improve the analytical accuracy.

The purpose of the utility model is realized through the following technical scheme:

the utility model provides a kind feeding chromatographic bottle for liquid chromatograph, includes bottle post, nut, column joint, seal cover, packing ring and pressure cap, nut and column joint are connected to bottle post lower extreme, and bottle post upper end forms sealing joint by seal cover, packing ring and pressure cap, sets up the sieve between sealing joint and the bottle post upper end, be used for filling the stationary phase granule in the bottle post, the bottle post inner wall evenly is provided with a plurality of little stings, little thorn size is unanimous with stationary phase granule size for little thorn pierces in the packing column that the stationary phase granule formed.

The traditional chromatographic column generally polishes the inner wall of the column to be very smooth in order to improve the smooth flow of a mobile phase, but in practical application, the smooth surface is not stably contacted with stationary phase particles, so that the mobile phase forms a channel flow on the surface of the stationary phase close to the inner wall of the column, and no filling process can solve the problem at present.

Furthermore, a protective layer made of the same material as the stationary phase particles is coated on the surface of the micro-pricks. The micro-thorns are designed to be made of the same material as the stationary phase, so that the influence of the micro-thorns on the liquid phase can be further eliminated.

Furthermore, the contact part of the micro-pricks and the inner wall of the bottle column is polished into a smooth surface.

Further, the sieve comprises flow distribution plate, filter screen and filter paper from top to bottom in proper order.

Furthermore, the splitter plate is annularly distributed and provided with a plurality of circles of arc-shaped notches. The design divides the traditional large-range liquid phase flow into layered liquid phase flow, thereby avoiding channeling of large flow streams.

The utility model has the advantages that:

(1) according to the scheme, the inner wall of the bottle column is provided with the micro-thorns with the same size as the stationary phase material and the particles, so that a plurality of fixed points are formed on the surface of the stationary phase, and the formation of channeling during flowing of the mobile phase can be avoided;

(2) the flow of the traditional single-strand liquid phase is divided into a plurality of strands by utilizing the flow distribution plate, and each strand has wide range and small thickness, so that the diffusion of the liquid phase in the stationary phase particles is delayed, and stable chromatographic analysis is obtained.

Drawings

FIG. 1 is a schematic structural view of the present invention;

FIG. 2 is an enlarged view of a portion of FIG. 1 at A;

fig. 3 is a schematic view of a screen deck stratification;

fig. 4 is a schematic view of a diverter plate configuration.

Detailed Description

The technical solution of the present invention is described in further detail below with reference to the accompanying drawings, but the scope of the present invention is not limited to the following description.

As shown in fig. 1, a sample introduction chromatographic bottle for a liquid chromatograph comprises a bottle column 1, a screw cap 2, a column joint 3, a sealing sleeve 4, a gasket 5, a pressure cap 6 and a sieve plate 9. The lower end of the bottle column 1 is connected with a screw cap 2 and a column joint 3, the upper end of the bottle column 1 is formed into a sealing joint by a sealing sleeve 4, a gasket 5 and a pressing cap 6, and the sealing joint is connected with a sample injection pipe 8 into the sealing joint through a connecting screw 7. A sieve plate 9 is arranged between the sealing joint and the upper end of the bottle column 1, so that a liquid phase sample is sent into the bottle column 1 through the sieve plate 9 through the sample inlet pipe 8. The bottle column 1 is filled with stationary phase particles, the inner wall of the bottle column 1 is uniformly provided with a plurality of micro-thorns 10, and the size of the micro-thorns 10 is consistent with that of the stationary phase particles, so that the micro-thorns 10 penetrate into the filling column formed by the stationary phase particles. Referring to fig. 2, which is an enlarged schematic view of the micro-prick 10, the surface of the micro-prick 10 is coated with a protective layer made of the same material as the stationary phase particles, and after the micro-prick 10 pierces the stationary phase particles, a plurality of stationary phase particle positioning points are formed on the surface of the solid phase filler, and these positioning points adsorb the surrounding stationary phase particles together, thereby avoiding the generation of channeling during the liquid phase flow. Preferably, the contact part of the micro-pricks 10 and the inner wall of the bottle post 1 is polished and polished to be smooth. As shown in fig. 3, the sieve plate 9 is composed of a splitter plate 91, a filter screen 92 and filter paper 93 from top to bottom. The structure of the splitter plate 91, which is designed in an annular shape and has a plurality of circles of arc-shaped notches 911, can refer to fig. 4, and the design can divide the liquid phase which originally flows in from one inlet into a plurality of liquid phase flows with arc-shaped end surfaces, thereby avoiding the filling bed from being flushed by a large amount of liquid phase.

The foregoing is illustrative of the preferred embodiments of the present invention, and it is to be understood that the invention is not limited to the precise forms disclosed herein, and that various other combinations, modifications, and environments may be resorted to, falling within the scope of the invention as defined by the appended claims. But that modifications and variations may be effected by those skilled in the art without departing from the spirit and scope of the invention, which is to be limited only by the claims appended hereto.

Claims

1. The utility model provides a kind feeding chromatographic bottle for liquid chromatograph, includes bottle post (1), nut (2), column joint (3), seal cover (4), packing ring (5) and pressure cap (6), nut (2) and column joint (3) are connected to bottle post (1) lower extreme, and bottle post (1) upper end is by seal cover (4), packing ring (5) and pressure cap (6) formation sealing joint, sets up sieve (9) between sealing joint and bottle post (1) upper end, be used for filling the stationary phase granule in bottle post (1), a serial communication port, bottle post (1) inner wall evenly is provided with a plurality of stings (10), stings (10) size is unanimous with stationary phase granule size for stings (10) pierce the packing post that the stationary phase granule formed.

2. The sample introduction chromatographic cylinder for the liquid chromatograph according to claim 1, wherein the surface of the micro-pricks (10) is coated with a protective layer made of the same material as the stationary phase particles.

3. The sample introduction chromatographic bottle for the liquid chromatograph according to claim 1, wherein the contact part of the micro-pricks (10) and the inner wall of the bottle column (1) is polished and polished to be smooth.

4. The sample introduction chromatography bottle for liquid chromatography according to any of claims 1 to 3, wherein the sieve plate (9) is composed of a splitter plate (91), a filter screen (92) and a filter paper (93) in sequence from top to bottom.

5. The sample introduction chromatography bottle for liquid chromatograph of claim 4, wherein the splitter plate (91) is configured with a plurality of circles of arc-shaped notches (911) distributed annularly.