JPH03197863A - Movable plug type column for liquid chromatography - Google Patents

Abstract

PURPOSE:To avert the damage of a sealing member at the time of device assembly by inserting the small-diameter part of a movable plug having a large- diameter part and the small-diameter part into a column body and providing a depressing means which makes sealing action in the large-diameter part. CONSTITUTION:The movable plug 3 inserted in the column body 1 has the large-diameter part 3a and the small-diameter part 3b connected to the outside of the body 1 and is formed with a small-diameter projecting part 3c in the peak part of the small-diameter part 3b. The projecting part 3c for fixing the movable plug 3 is fitted into the central hole of a retaining disk 13. A recess 3d fitted with a liquid dispersing plate 16 is provided at the bottom end face of the large-diameter part 3a of the movable plug 3 and a liquid passage path 15 penetrated from the center of the recess 3d to the front end of the projecting part 3c is formed. The disk 13 is moved relative to the flange 1b by tightening a fastening bolt 5, by which the movable plug 3 is moved downward. In addition, the packing material 2 in the column 1 is depressed by the bottom end of the movable plug 3, by which the sealing device is assembled without damaging the sealing member 6.

Description

Detailed Description of the Invention (Industrial Field of Application) The present invention relates to a movable stopper column for liquid chromatography, and more specifically, a movable plug column for sealing the inside of the column from the outside at the sliding surface between the movable stopper and the column body. This relates to a sealing structure.

(Prior Art) Generally, movable stopper columns for liquid chromatography are used in a wide range of industrial fields such as the food manufacturing industry and the pharmaceutical manufacturing industry to separate and recover useful components from a fluid containing them.

This liquid chromatography device collects a fraction enriched with a specific component by passing a raw material fluid through a packing material packed in a column, and the packing state of the packing material greatly affects its separation performance. It is well known to do. For example, if a top-off phenomenon (referred to as "interval II occurrence") occurs in the filler layer due to various factors such as usage conditions and frequency, the separation performance will be greatly reduced.

Therefore, recently, a movable stopper column for liquid chromatography has been proposed as an apparatus having a function to deal with such problems.

This movable plug type column device has a structure in which the upper part of the column body is closed by a movable plug that can be moved up and down. Therefore, the above-mentioned top-off phenomenon (11
! The feature is that when a problem occurs, it can be recovered and stabilized by pressing the filler layer by moving the movable stopper downward.

The conventional structure of a movable stopper column for liquid chromatography that has such a function is that a movable stopper is installed inside the column body so that it can move up and down at the top of the column, and the movable stopper is moved downward from the outside to fill the column. After pressing down the drug layer, it is fixed to the column body by a movable stopper fixing means.

The means for fixing the movable stopper is, for example, by arranging disk-shaped movable stopper flanges facing each other above the upper flange of the column body, and connecting the upper flange and the moveable stopper flange with a number of fastening bolts. It is common to have a structure in which the movable stopper is moved downward by tightening, thereby exerting a downward action on the filler layer. Furthermore, in order to prevent seal leakage between the movable stopper and the circumferential surface of the column body, a sealing device is usually provided that seals the movable stopper by fitting a seal member into the circumferential groove of the column body.

(Problems to be Solved by the Invention) The above-mentioned movable stopper column for liquid chromatography is intended to solve the above-mentioned problems such as the top-off phenomenon of the lid packing layer during use. However, since the column is used under pressure, if liquid leaks due to deterioration of the sealing performance of the sealing device, separation performance may deteriorate significantly or useful substances may leak out of the column due to liquid leakage. There is a problem in that the device may not be able to perform its original function as a liquid chromatography device due to dissipation.

According to the inventor's study of this problem, one of the causes of seal failure is that when the movable stopper is moved down relative to the column body and further pushed down against the packed bed, multiple tightening Even if the bolts are tightened in an appropriate manner, they tend to become loose, which may cause deterioration of the sealing member and cause liquid leakage after long-term use.

This problem becomes a serious problem because it is difficult to tighten evenly, especially in large-scale equipment with a diameter of several tens of centimeters used on an industrial scale.

Therefore, if such sealing failure occurs in the sealing device, it is necessary to repair the sealing device, but in conventional devices, to repair this, the movable stopper is pulled out from the column body and the sealing member is removed. It is necessary to replace it and insert it into the column again. However, this work must be done carefully to avoid disturbing the filler layer, is complicated, and requires a high degree of skill from the operator, making it difficult.
There was also considerable equipment downtime and expense burdens.

The present invention has been made in view of these problems, and its purpose is to eliminate problems such as damage to the sealing member during device assembly, and to enable easy assembly of the sealing device. An object of the present invention is to provide a movable stopper column for liquid chromatography.

Another object of the present invention is to provide a liquid chromatography system with a structure that allows repair of only the sealing device without removing the movable stopper from the column body in the event that a seal leakage problem occurs in the sealing device. An object of the present invention is to provide a movable stopper type column for use in photography.

(Means and effects for solving problem a) A feature of the movable stopper column for liquid chromatography according to the present invention to achieve the above object is that it is movable in the vertical direction within the upper cylinder of the column body. a sealing device that seals the inside of the column from the outside by inserting a ring-shaped sealing member between the opposing peripheral surfaces of the column body and the movable stopper; and a sealing device that seals the interior of the column from the outside; In the movable stopper type column for liquid chromatography, the sealing device is provided with a movable stopper fixing means for fixing with a movable stopper, and the sealing device has an annular stopper that supports the ring-shaped sealing member and has substantially no gap with respect to the inner circumferential surface of the column body. The movable stopper is provided in a stepped manner so as to have a large diameter part having the supporting upper surface on the outer periphery, and a small diameter part that continues from the large diameter part to the outside of the column body, and A pressing means is provided which is fitted into the column body from above and clamps the sealing member together with the supporting upper surface of the large diameter portion to exert a sealing action, and furthermore, this pressing means is removable from the column body. In addition, the movable stopper is configured to be fixed to either the movable stopper or the movable stopper fixing means.

By having the above-described structure, the device of the present invention does not cause damage to the sealing member when moving the movable stopper downward or pressing down the filler layer, and it is possible to add, replace, or repair the sealing device to the moveable stopper. It can be done while it is fixed.

Note that the seal member used in the above configuration is typically a type that can be removed and assembled in the radial direction from the movable stopper, such as a bias cut type seal ring or a spiral type seal ring. However, it is not particularly limited to this.

(Example) The present invention will be described below based on embodiments shown in the drawings.

FIG. 1 is a diagram showing an outline of the structure of a movable stopper column for liquid chromatography according to the present invention, in which 1 is a cylindrical column body with both upper and lower ends open, and a lower flange 1a is provided at the lower end of the column body. An upper flange 1b is provided at the upper end.
is provided. The lower flange 1a has a plurality of fastening bolts 10 (only one bolt is shown in the figure).
The lower lid 9 is fastened and fixed, thereby partitioning the inside of the column from the outside and allowing a predetermined liquid to flow between the column and the outside through the liquid passage 12 formed in the center of the lower lid 9. There is.

It should be noted that a sealing portion in which a sealing member (not shown) is assembled is provided on the engagement surface of the lower flange 1a and the lower lid 9 to provide airtight sealing and sealing with the outside. Moreover, 11 is a fruit plate.

Reference numeral 3 denotes a movable plug housed inside the upper side cylinder of the column body 1, and its lower end has a large diameter portion 3a having an outer diameter slightly smaller than the inner diameter of the column body, and a sealing member that is larger than the large diameter portion 3a. The assembly has a small diameter portion 3b having a small diameter, and this small diameter portion 3b is formed to protrude sufficiently long from the upper part of the column body. The top of this small diameter portion 3b is formed as a convex portion 3C having a smaller diameter.
c is the center hole 13a of the presser disk 13 for fixing the movable stopper.
The mating is fixed.

Also, a liquid dispersion plate 1 is provided on the lower end surface of the large diameter portion 3a of the movable stopper 3.
6 is fitted into the recess 3d, and this recess 3
A liquid passage 15 is formed passing through the center of the shaft from the center of d to the tip of the convex portion 3c.

The presser disk 13 is connected to the upper flange 1b of the column body 1 by a plurality of fastening bolts 5 (only one is shown in the drawing), and these fastening bolts 5, the presser disk 13 is moved relative to the lower flange 1b, thereby moving the movable plug 3 downward, and the lower end of the movable plug 3 can press down the packing layer 2 in the column. ing.

The above configuration is substantially the same as a conventional movable stopper column for liquid chromatography, except for the shape of the moveable stopper 3.

The feature of this embodiment is that a sealing device is formed in the following manner in relation to the shape of the movable stopper 3 described above.

That is, the stepped portions of the large diameter part 3a and the small diameter part 3b of the movable stopper 3 provide an annular supporting upper surface 3e for supporting the sealing member on the ring, and on this supporting upper surface 3e, the sealing member 6, for example, is mounted on a bias. A cut seal ring is fitted. In this example, the sealing member 6 does not exhibit a sealing effect when simply fitted between the inner peripheral surface of the column body 1 and the small diameter portion 3b of the movable stopper 3; There is no problem even if it exhibits a certain degree of sealing effect even when the seal is closed.

Reference numeral 8 denotes an annular bearing plate placed on the upper part of the seal member 6, and the tightening described later is for applying a pressing edge to the seal member 6 evenly by means of the nut member 14. In this example, the bearing plate 8 is divided into two or more parts in the circumferential direction so that it can be removed in the radial direction from the movable stopper 3, but the sealing member 6 can be replaced. In this case, it is not necessary that the bearing plate 8 itself be removable in the radial direction with respect to the movable stopper 3.

Numeral 14 is a tightening nut member, which is attached to the small diameter portion 3b of the movable stopper 3.
is screwed into the male threaded part 3f formed on the upper part of the screw, and when the screw rotates downward, it provides a pressing edge to the sealing member 6 via the bearing pressure plate 8, and conversely, when the screw rotates upward, the sealing member 6 It is designed to release the pressed blade against. This tightening is done because the lower end of the nut member 14 can be pulled out from the column body by upward screw rotation, and the bearing plate 8 and seal member 6 can be taken out from the outside. The dimensional relationship, such as the screw length, is set.

The assembly and removal of the sealing device having the above configuration will be explained.

At the time of initial assembly, for example, the movable stopper 3 is inserted into the column body 1 and the seal member 6 is inserted at the same time, and the bearing pressure plate 8 is inserted into the column body 1.
is placed on the seal member 6, and tightened by screwing the nut member 14 together. In this state, the presser disc 13 is attached to the upper part of the movable stopper 3, and the movable stopper 3 is moved downward by tightening the fastening bolt 5, so that a predetermined push-down blade acts on the filler layer.

Thereafter, the nut member 14 is screwed in until a predetermined sealing effect can be exerted, thereby completing the assembly work of the sealing device.

In this example, if it is necessary to move the movable stopper 3 downward to press down on the filler layer because a top-off phenomenon occurs between the liquid dispersion plate 16 and the filler layer as a result of use. By tightening the fastening bolt 5, the nut member 14 is also moved simultaneously with the movable stopper 3.

When inspecting or replacing the seal member 6, loosen the nut member 14, take out the seal member 6, perform the necessary inspection or replacement, insert a new seal member 6, and tighten the nut member. The work is completed just by screwing in 14.

FIG. 2 is for explaining another embodiment of the present invention, and the embodiment shown in this figure has completely the same structure as the example shown in FIG. 1 except that the structure of the sealing device is different. It consists of
Therefore, the same members are given the same reference numerals and their explanations will be omitted.

In the sealing device of this embodiment, a screw rod 7 is screwed through a through screw hole 13b (out of a plurality of holes provided in the circumferential direction, only one is shown in the drawing) provided in a presser disk 13, and this screw rod By screwing in, a pressing edge is provided to the sealing member 6 via the bearing pressure plate 8.

(Effects of the Invention) As explained above, in the movable stopper column for liquid chromatography of the present invention, the movable stopper can be assembled to the column body and the original sealing function can be easily exerted after the movable stopper is fixed. This has the effect of avoiding problems such as damage to the sealing member during device assembly.

In addition, if a problem with the sealing edge occurs in the sealing device, the sealing function can be quickly restored by adding or replacing only the sealing device, without removing the movable stopper while it is fixed to the column body. Especially in the case of equipment used on an industrial scale for diagnostic purposes, it has the effect of significantly reducing the significant drop in productivity due to equipment stoppages, etc., and is extremely useful.

[Brief explanation of drawings]

Figure 41 is a diagram showing an outline of the configuration of a movable plug column for liquid chromatography according to the present invention - an example, and Figure 2 is a diagram showing an outline of the configuration of a movable plug column for liquid chromatography according to another embodiment. It is. 1: Column body 2: Filler layer 3: Movable stopper 5: Tightening bolt 6; Seal member 7: Tightening bolt 8: Bearing plate
14: Tightening was done by nut members and 4 other people.

Claims (1)

[Scope of Claims] 1. A movable stopper that is internally movable in the vertical direction in the upper side cylinder of the column body, and a ring-shaped seal member inserted between the opposing peripheral surfaces of the column body and the movable stopper. A movable stopper column for liquid chromatography that is provided with a sealing device that seals the inside of the column from the outside, and a movable stopper fixing means that fixes the movable stopper at a predetermined position relative to the column body, the sealing device comprising: A large diameter portion having substantially no gap with respect to the inner circumferential surface of the column body and having an annular supporting upper surface supporting the ring-shaped seal member on the outer circumferential edge, and a small diameter portion continuing from the large diameter portion to the outside of the column body. The movable stopper is provided in a stepped manner so that the moveable stopper has a stepped small diameter portion, and is inserted into the column body from around the stepped small diameter portion of the movable stopper, and pinches the sealing member with the supporting upper surface of the large diameter portion to perform a sealing action. A liquid chromatograph, characterized in that it is provided with a push-down means for exerting the force, and the push-down means is provided so as to be removable outside the column body and fixed to either the movable stopper or the movable stopper fixing means. Movable stopper column for graphics.