JPH0843373A - Movable plug type liquid chromatographic column - Google Patents

Abstract

PURPOSE:To provide a column for liquid chromatography of movable plug type with which filling column can be removed from a pressurizing device just after the filling of a filler material is completed. CONSTITUTION:A column for liquid chromatography is structured so that a movable plug 31 having a flow path capable of being opened and closed is slidably inserted in a shell 11 which is for filling of a filler material and has at one end a flow path 26 capable of being opened and closed, wherein a nut- shaped hub 40 is fitted on a bolt-shaped piston rod 37 connected with the back face of the plug 31 and is secured to the upper flange 13 of the shell 11 by a locking means R2.

Description

Detailed Description of the Invention

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a movable stopper type liquid chromatography column, and more particularly, to a movable stopper type liquid chromatography column capable of separating a column from a pressurizing device upon completion of filling with a packing material. About.

[0002]

2. Description of the Related Art A conventional column for industrial high performance liquid chromatography is provided with flanges provided at both ends of a shell, and a separating agent is filled with a dry type or after a slurry is charged into a shell connected to a slurry reservoir. This is done by feeding a solvent and applying pressure. In addition, the separating agent was filled with the shell at both ends, and was fixed with a flange type lid having a filter.

Therefore, in these two filling methods, it is impossible to fill the separating agent having a small particle size, or the separating agent performance cannot be sufficiently exhibited.

[0004] On the other hand, a movable shaft type column has been developed to enable a large-diameter (50 mm or more inner diameter) column for industrial high-performance liquid chromatography to be packed with a separating agent having a small particle size. The (100 bar / square centimeter) movable shaft column was integral with the pressurizing device and the packed column could not be removed.

[0005]

SUMMARY OF THE INVENTION The present invention has been made in view of the above-mentioned problems of the prior art, and a movable plug type liquid in which the packed column can be removed from the pressurizing device as soon as the packing of the packing material is completed. It is intended to provide a column for chromatography.

Another object of the present invention is to provide a movable stopper type liquid chromatography column in which the mechanism for fixing the movable stopper at a fixed position is extremely simple and its operation is easy.

[0007]

According to the present invention, there is provided a movable plug in which a movable plug having an openable / closable passage is slidably inserted into a filler filling shell having an openable / closable passage at one end. In a column for liquid chromatography, a nut-shaped hub is screwed onto a bolt-shaped piston rod connected to the back surface of the movable stopper, and the hub is fixed to a flange of the shell by a locking means. The present invention provides a movable stopper type liquid chromatography column.

As the locking means, a plurality of clamps having an inner groove on the inner surface sufficient to fit the flanges of the hub and the shell in contact with each other, and provided at both ends of each clamp. It is preferable for use to be formed from a clamp connecting lug.

[0009]

[Function] After the filler filled in the shell is pressed until the pressure of the movable plug reaches the set load weight, the nut-shaped hub screwed to the bolt-shaped piston rod connected to the back surface of the movable plug is Turn to join the flange of the shell. Then, when the hub is fixed to the flange of the shell by the locking means, the movable plug does not move back, so that the shell, in other words, the column can be removed from the pressurizing device.

[0010]

Embodiments of the present invention will be described below with reference to the drawings. In this embodiment, a case in which a half-split type clamp is used as the locking means is taken as an example.

In FIG. 1, reference numeral 10 denotes a movable stopper type liquid chromatography column. A main body of the column 10, that is, a cylindrical shell 11, has a lower flange 12 for attaching a cover at one end thereof and another end thereof. And a setting flange 14 for attaching the shell 11 to the column set stage 1 of the packing apparatus.

A cover 21 on which a liquid collecting plate 22, a lower filter 23, and a polytetrafluoroethylene (PTFE) sleeve 24 are set is detachably attached to the lower flange 12 by a lower locking means R1 described later.

At this time, in the outer peripheral groove 15 at the bottom of the shell, P
The seal ring 25 made of TFE is incorporated. In addition, a plug 27 is provided in the flow path hole (flow path) 26 provided in the central portion of the cover 21.
Attach. On the other hand, as shown in FIGS. 1 and 2, the dispersion plate 32 and the upper filter 33 are pushed into the movable plug 31 inserted into the shell 11 together with the sleeve 34 made of PTFE to be fixed. Further, a PTFE seal ring 36 is attached to the outer peripheral groove 35 of the movable plug 31 to prevent liquid leakage.

In the head outer peripheral groove 38 of the bolt-shaped piston rod 37 which is bolted to the back surface of the movable stopper 31,
A slide ring 39 made of PTFE is attached in order to smooth the sliding movement of the movable plug 31.

Further, a nut-shaped blind hub 40, a lock nut 41 and a connecting board 42 are sequentially screwed and attached to the bolt-shaped piston rod 37. At this time, the surface of the connection board 42 and the upper end of the piston rod 37 are
Match on the same side.

A pipe (flow path) 44 passed through a pipe 43 provided at the axis of the piston rod 37 is attached to the movable plug 31 by a pipe screw 45. An open / close valve (not shown) is attached to the pipe 44.

When the blind hub 40 is fixed to the upper flange 13 of the shell 11 as shown in FIG.
Use 2. The upper locking means R2 is shown in FIGS.
, Two arc-shaped clamps 51 and 53 and connecting lugs 52 and 53 fixed to both ends thereof, respectively.
54.

The lugs 54 attached to the clamp 52 are vertically arranged in two stages, and sandwich the lug 52 of the clamp 51 from above and below as shown in FIG. Further, as can be seen from FIG. 5, the clamp 51 has a groove 55 on the inner side surface, and the height (thickness) thereof is almost the same as the total thickness of the blind hub 47 and the upper flange 13, or more than that. It is slightly higher. Further, the clamp 53 is formed in the same shape as the clamp 51.

Since the lower locking means R1 has the same structure as the upper locking means R2, a detailed description is omitted. However, in the case of the lower locking means R1, the height (thickness) of the groove 55
Is approximately equal to or slightly higher than the total thickness of the lower flange 12 and the flange 28 of the cover 21.

Next, the assembly and operation of the column will be described. After the cover 21 on which the liquid collecting plate 22, the lower filter 23, and the sleeve 24 are set is attached to the lower portion of the shell 11, as shown in FIG.

Further, as shown in FIG. 6, the piston rod 37 to which the movable stopper 31 is attached is fastened to the connecting plate 3 of the pressurizing device 2 via the connecting board 42 with bolts. Then shell 11
A slurry liquid in which a filler is dispersed in a solvent is poured into the inside (not shown).

Next, the oil jack 2 which is a pressurizing device.
When the pressurizing shaft 4 is lowered, the movable plug 31 is inserted into the shell 11, and when the solvent starts to be discharged from the tube 44 attached to the movable plug 31, the movement of the pressurizing shaft 4 is stopped and the valve of the tube 44 is opened. close.

Next, the stopper 27 of the cover 21 is removed, and the pressure shaft 4 is lowered. When the discharge of the slurry solvent from the flow path hole 26 of the cover 21 is completed, the pressurization pressure is raised to an arbitrary pressure and stopped at that pressure. Then, a stopper 27 is inserted into the flow passage hole 26 of the cover 21.

Next, as shown in FIG. 7, the blind hub 40 is screwed until it comes into contact with the shell 11, then the blind hub 40 and the upper flange 13 are sandwiched by a pair of clamps 51, 53, and the lugs 52, 54 are bolted to each other by bolts 60. , 60. Further, the lock nut 41 is tightened.

Next, as shown in FIG. 8, the bolts which fasten the connecting plate 3 of the pressurizing device and the connecting plate 42 of the movable plug 31 are removed, the pressurizing shaft 4 is raised, and the shell 11 is moved to the column set stage of the filling device. Remove from 1.

As described above, in the present invention, the mechanism for fixing the movable stopper 31 at an arbitrary position is extremely simple, and the operation thereof is easy. Further, according to the present invention, the movable stopper 31 is always fixed at the initially set pressure and position, so that the sample separation effect is optimally maintained. Further, according to the present invention, since the shell 11 (column body) can be removed from the pressurizing device 2, only the shell 11 can be moved.

Although the embodiments of the present invention have been described above, the specific configuration is not limited to these embodiments, and the present invention can be applied even if there is a design change or the like without changing the gist of the present invention. included. That is, a fastening bolt may be used for the locking means. However, at that time, the bolt hole provided in the blind hub needs to be an arcuate hole that follows the circumferential direction of the blind hub, and uneven tightening may occur.

[0028]

As described above, according to the present invention, the mechanism for fixing the movable plug at an arbitrary position is extremely simple, and its operation is easy. Further, in the present invention, since the movable stopper is always fixed at the initial pressing and position, the sample separation effect is optimally maintained. Further, according to the present invention, since the shell (column body) can be removed from the pressurizing device, only the shell can be appropriately moved.

[Brief description of drawings]

FIG. 1 is a side view including a partial cross section of a movable stopper type liquid chromatography column according to the present invention.

FIG. 2 is a sectional view of a main part of a movable stopper type liquid chromatography column according to the present invention.

FIG. 3 is a plan view of one of two divided clamps.

FIG. 4 is a plan view of another one of the two clamps.

FIG. 5 is a front view taken in the direction of arrows VV in FIG. 3;

FIG. 6 is an explanatory diagram showing a state in which a shell is attached to a column set stage of a filling device and a movable stopper is attached to a connection plate of a pressurizing device.

FIG. 7 is an explanatory diagram showing a state in which a blind hub is fixed to a shell by a clamp.

FIG. 8 is an explanatory view showing a state in which a movable stopper is removed from a connection plate of the pressurizing device.

[Explanation of symbols]

 DESCRIPTION OF SYMBOLS 10 Column 11 Shell 13 Upper flange 26 Flow path hole (flow path) 31 Movable stopper 37 Piston rod 40 Hub 44 Pipe (flow path) R2 Locking means

Claims (2)

[Claims] 1. A movable plug type liquid chromatography column having a movable plug having an openable / closable flow path slidably inserted into a filler filling shell having an openable / closable flow path at one end, A nut-shaped hub is screwed into a bolt-shaped piston rod connected to the back surface of the movable plug, and the hub is fixed to a flange of the shell by locking means. column. 2. Locking means are provided at a plurality of clamps having an inner groove on an inner surface sufficient to fit into a flange of a hub and a shell in contact with each other, and at both ends of each clamp. The movable plug type liquid chromatography column according to claim 1, wherein the column is formed from a clamp connecting lug.