JPS6243568A - Chromatography apparatus - Google Patents

Abstract

PURPOSE:To obtain a backed column with a high pressure filling effect maintained, by sticking a tip body of a piston-shaped cap out of a rear end body thereof to make a filler compacted into the backed column repressurizable. CONSTITUTION:A cap 14 having a porous plate 12 is mounted at one end of a backed column 10 packed with a filler. The porous plate 12 is made of material such as sintered material that allows a fluid of liquid or gas alone to pass but does not do the filler. A cylinder-shaped cap 16 divided into a tip body 18 and a rear end body 20 is inserted from the other end of the backed column 10. Then, after the column 10 is packed with the filler, the cap 16 is retained on the inner wall surface of the column 10 by pressing taperings 42 and 44 of the rear end body 20 with a holding ring 46. The tip body 18 sticks out of the rear end body 20 by an oil pressure introduced from an oil pressure introduction hole 36 to repressurize the filler.

Description

Detailed Description of the Invention [Field of Industrial Application] The present invention relates to a chromatography apparatus such as liquid chromatography, gas chromatography, or supercritical chromatography, and in particular, the present invention relates to a chromatography apparatus such as liquid chromatography, gas chromatography, or supercritical chromatography. This relates to a chromatography device a that can be pressurized.

[Prior Art] Liquid chromatography and gas chromatography are known as devices for separating specific components from solutions and mixed gases. As is well known, this chromatography equipment uses a chromatography column filled with a packing material of microparticle size, and the chromatography column is packed with packing material densely and uniformly, resulting in superior performance. It is possible to exhibit excellent separation performance. Traditionally, high-pressure packing of packing materials into chromatography columns requires
A method is used in which a filling bag W (for example, a high-pressure pump) is connected to a chromatography column, high-pressure filling is performed, and a removal stopper is attached to a pre-filling device after filling.

Also known is a method in which a piston is inserted into a chromatography column, and the slurry of the packing material introduced into the column is 61ii and compacted by the piston (Japanese Patent Publication No. 58-20284).

[Problems to be Solved by the Invention] Among the conventional filling methods described above, in the method using a filling device such as a high-pressure pump, if it becomes necessary to increase the filling pressure after filling the filling material, , it is necessary to remove the stopper, replenish the filling material, and repressurize. Therefore, even if the filling pressure of the filling material decreases or the filling state becomes uneven,
It was difficult to take a quick response. Further, in this conventional method, when attaching the stopper, the packing device is removed from the chromatography column and then the stopper is attached, so there is a problem that the filling pressure of the packing material is released for a long time.

In other words, the purpose of high-pressure packing in a column is to obtain a column with high separation efficiency, but even if high-pressure packing is performed, if the packing pressure is released for a long time before plugging, the packing density will vary. occurs, and the effect of high-pressure filling becomes smaller. In relatively small-diameter columns, the packing pressure is relatively easily maintained due to the bleed phenomenon of the packing material, but the larger the diameter, the greater the degree of release of the packing pressure when the packing device is removed. The effect of high pressure filling is reduced.

In addition, when inserting a piston into a chromatography column to perform high-pressure filling as in Japanese Patent Publication No. 58-20284, it is possible to pressurize the packing material again, and the effect of high-pressure filling can be maintained. is also possible. However, since the chromatography column and the pressurized packing device are always integrated, the entire chromatography device becomes large and requires a large installation space, and the cost of the device is also high.

[Means for Solving the Problems] The chromatography apparatus of the present invention has a chromatography column closed at both ends with a cap having a perforated plate through which a fluid can pass, and a packing material is placed inside the chromatography column. In the cap 2 on the one end side, the cap 2 is divided into a tip end body and a rear end body. Then, this rear end body is secured to a chromatography column. As this engaging W means, one that can be engaged with the inner wall surface of the chromatography column by protruding its side peripheral surface is used. Further, a pressing means is provided for causing the tip end body to protrude from the rear end body. Hereinafter, the column filled with this packing material will be referred to as a back column, and the cap that slides inside the back column will be referred to as a piston-shaped cap.

[Operation] In the chromatography apparatus of the present invention, by causing the leading end to protrude from the trailing end, the packing material already packed in the back column at high pressure can be pressurized again.

Moreover, in the chromatography apparatus of the present invention.

A slurry of filler is introduced into the back column and is pressed by the piston-shaped cap, and then the side circumferential surface of the rear end of the piston-shaped cap is made to protrude, and can be latched to the inner wall surface of the back column as it is. Therefore, according to the present invention, it is possible to maintain the pressure at the time of filling the back column.

Furthermore, after filling, the backed column can be separated from an attached packing device, such as a piston-shaped cap pushing device, so that the configuration of the chromatography device during use can be simplified.

[Example] Examples will be described below with reference to the drawings.

FIG. 1 is a longitudinal sectional view of a chromatography apparatus according to an embodiment of the present invention. In FIG. 1, the symbol IO is a back column loaded with a packing material, and the symbol A is a packing material layer packed in this column. One end of this backed column 10 (
(upper end in the figure) is a cap 14 having a perforated plate 12.
is installed. Note that the porous plate 12 is made of a material such as sintered metal or porous ceramic that allows only a liquid or gaseous fluid to pass through, but not a filler. The cap 14 is a clamp 15 in this embodiment.
Although this is connected to one end of the backed column 10, the backed column 10 and the cap 14 may be provided with flanges and connected by bolts.

A piston-shaped cap 16 is inserted from the other end of the backed column 10 (lower end in the figure).

Next, an example of the structure of the piston-shaped cap 16 will be described with reference to FIGS. 2 to 6.

The piston-like cap 16a shown in FIG.
and a rear end body 20. In the attitude shown in FIG. 2, the upper surface of the tip body 18 is shallowly hollowed out to form a recess 22, and the perforated plate 1 is placed over the recess 22.
2 is fixed. Further, a communication hole 24 is provided to communicate the four parts 22 with the opposite side of the piston-shaped cap 16a.
is bored in the axial direction of the tip body 18. Tip body 1
8, a thick cylindrical plunger-shaped protrusion 26 is bored on the lower surface side. Further, a seal ring 28 is wound around the side peripheral surface of the tip body 18, and this seal ring is attached to a scraper part 30 that is a part of the seal ring.
and is fixed by a cheat 32 screwed onto the tip body 18.

On the other hand, the rear end body 20 is provided with a cylindrical recess 34 in the shape of a circumferential groove into which the plunger-like protrusion 26 is inserted. Between these convex parts 26 and concave parts 34, the rear end body 2
Hydraulic pressure can be introduced from a hydraulic pressure introduction hole 36 provided at 0. Reference numerals 38a and 38b are O-rings that perform hydraulic sealing.

Further, reference numeral 40 denotes a center hole of the rear end body 20, which is provided coaxially with the communication hole 24.

A cap fixing tapered ring 42, 44 and a tapered ring holding ring 46 are attached to the side peripheral surface of the rear end body 20.

The tapered rings 42 and 44 for fixing the cap have slopes 42a and 44a that slide against each other.
4 upward in the figure, the retaper ring 42 bulges out, and it is possible to lock the rear end body 20 to the inner wall surface of the back column IO. In the example shown in FIG. 2, the screw 48 is inserted through the retaining ring 46 and
When this screw 48 is tightened, the taper ring 44 is pressed and moved by the taper ring holding ring 46 so as to slip into the inside of the taper ring 42, and the taper ring 42 is pressed against the side periphery of the rear end body 20. It can bulge out of the surface.

In the piston-like cap 16b of FIG. 3, tapered rings 50, 52 are used.

As shown in FIG. 4, the tapered ring 50 is a ring having a trapezoidal cross section, the height of which is smaller on the outer circumferential side than on the inner circumferential side, and is inserted into the rear end body 20. On the other hand, the tapered ring 52 is a ring with a trapezoidal cross-section whose height is smaller on the inner circumferential side than on the outer circumferential side.
They are arranged on the outer periphery side at a predetermined interval from 0.

As shown in FIG. 3, different taper rings 54 and 56 are installed to sandwich these taper rings 50 and 52, and the slopes of each of the taper rings 50 to 56 are set at an inclination angle that allows sliding. ing.

A bolt 58 is inserted through the taper ring 56, and the tip of the bolt 58 is screwed into the taper ring 54. Therefore, when the bolt 58 is tightened, the taper ring 54.
56 is moved in the approach direction, whereby the tapered ring 52 protrudes from the side surface of the rear end body 20b in a bulging manner.

In the piston-shaped cap 16c shown in FIGS. 5 and 6, four contact members 60 are provided. The abutting member 60 is a piece-shaped member having an outer peripheral surface curved in a circular arc shape as shown in FIG. It is attached to the body 20. Further, the outer peripheral surface of the contact member 60 is made of, for example, hard rubber, which has a large frictional resistance. Furthermore,
An arm 64 is pivotally supported at both ends by the abutting member 60 and the rear end body 20. This arm 64 is inclined upward toward the center of the rear end body 20 in the illustrated attitude. When this piston-shaped cap 16c is moved upward in the figure, the arm 64 receives the force of rotation in the direction of the arrow θ, and the friction force between the contact member 60 and the inner peripheral surface of the back column 10 or the filling column to be described later is reduced. The weakened piston-like cap 16c can slide smoothly inside the parked column IO or packed column. On the other hand, when the piston-shaped cap 16c receives a downward force in the figure, the arm 64 rotates in the counter-θ direction, the frictional force between the contact member 60 and the inner peripheral surface of the back column 10 or the packing column increases, and the piston A shaped camp 16c is secured to the inner peripheral surface.

The other configurations of the piston-shaped caps 16b and 16c are the same as that of the piston-shaped cap 16a, so the same members are given the same reference numerals and their explanations will be omitted.

In addition, as the rear end body 20 of the piston-shaped cap 16,
In short, it may have any structure as long as it can be reliably engaged with the back column IO, and may have a structure other than that shown in FIGS. 2 to 6.

Next, with reference to FIGS. 7 and 8, the back column lO
An example of a method for high-pressure filling a filler into the inside will be described.

In FIG. 7, the backed column 10 has a packing device 66
It is placed above. At the lower end of the backed column 10,
A flange 10a is provided, and this flange 10a
is connected to the fixed flange 68 by a clamp 70.

The fixed flange 68 is fixed to a support base 74 via a fixed rod 72, and the support base 74 is installed by legs 76 to maintain a horizontal position. The fixed flange 68 is provided with a through hole 78 having a diameter equal to or larger than the outer diameter of the backed column IO, and the backed column 10 is installed coaxially with this through hole 78.

Support base 74 and fixed flange 68 (7) ft+'
A packing column 80 having an inner diameter approximately equal to that of the backed column 10 is installed in the column 1. This packing column 80 is connected to a mounting base 82, and this mounting base 82 is moved up and down by a small junk 84. The small shirt J+84 is fixed to the support base 74, and its piston rod 84a extends upward, and its tip is fixed to the lower surface of the mounting base 82.

A flange 80a is provided at the upper end of the packing column 80, and this flange 80a is freely connected to the fixed flange 68 by a clamp 86. Note that the packing column 80 is located coaxially with the backed column 10.

Reference numeral 88 is a main jack fixed to the support base 74, and the piston rod 88a of the main jack 88 presses and moves the piston-shaped cap 16 from the lower end position of the filling column 80 to the lower end insertion position of the backed column IO. It has a stroke amount that can be used.

Next, a procedure for loading a filling material using the filling device 66 shown in FIG. 7 will be described.

First, the rod 88a of the main jack 88 is retracted to below the lower end of the filling column 80, and the piston-shaped caps 16 with adjusted seal rings 28 are inserted into the five filling columns 80, and the rod 88a I support it.

Thereafter, the clamp 15 is released, the cap 14 is removed from the L end of the backed column 10, and the slurry liquid of the packing material is injected into the backed column 10 and the packing column 80. After a predetermined amount of injection is completed, the camp 14 is placed over the back column 10 and fixed with a clamp 15. Then, the main jack 88 is operated to project the rod 88a and gradually move the piston-shaped cap 16 upward. Note that the communication hole 40 of the rear end body 20 of the piston-shaped cap 16 is closed with a blind plug (not shown), so that the liquid in the slurry liquid is not drained when the slurry liquid is injected and when the top A of the piston-shaped cap 16 is operated. This prevents any leakage from the piston-like cap 16.

The piston-like cap 16 is further pushed up and inserted into the lower end of the backed column 10. Then, the pressure of the compacted filler and the jack is balanced and the piston automatically stops.

Next, after releasing the clamp 86, the small jack 84 is operated to retract the rod 84a, and the packing column 8
0 gradually downwards.

After this, if the piston-shaped cap 16 has the configuration 16a or 16b shown in FIG. 5S2 or FIG.
8 or port 58 to lock the rear end body 20 to the inner wall surface of the backed column 10. (If the piston-like cap 16 has the configuration shown in FIG. 5, such screw or bolt tightening work is not necessary.) Thereafter, by releasing the clamp 70, a backed column 10 filled with the filler material is obtained. be able to.

The thus obtained backed column 10 maintains the high pressure packed by the main jack 88 without ever releasing it, so it maintains a uniform high pressure packed state.

FIG. 8 is a longitudinal sectional view showing the configuration of a different filling device, and the filling device in FIG. 8 has a configuration in which the filling device in FIG. 7 is turned upside down.

In the apparatus shown in FIG.
is supported on the inner circumference of the The flange lOa of the backed column 10 and the flange 80a of the packing column are removably connected by a clamp 92.

In the apparatus shown in FIG. 8, the leg portion 76 is omitted and a fixed base 94 is installed in its place, and the backed column 10 is erected on the fixed base 94. Further, the fixed rod 72 connects the fixed base 94 and the support base 74, and maintains a constant distance therebetween. Further, the tip (lower end in the figure) of the rod 88a of the main jack 88 is in contact with the upper surface of the rear end body 20 of the piston-shaped cap 16.

The rest of the configuration of the device in FIG. 8 is the same as that in FIG. 7 except that it is upside down, so the same members are given the same reference numerals and their explanations will be omitted.

Next, a procedure for loading a filler using the apparatus shown in FIG. 8 will be described.

First, the rod 88a of the main jack 88 is retracted and operated to extract it to the outside of the packing column 80. Next, the slurry liquid of the packing material is injected into the back column 10 and the packing column 80 from the upper part of the packed column 80. After injecting a predetermined amount of filler slurry liquid, the seal ring 28
Filling column 80 with piston-like cap 16 adjusted to
the rod 88a of the main jack 88 to protrude. Then, move the piston-shaped cap 16 downward,
Insert it into the packed column 80 and gradually push it further downward. This pressing down gradually consolidates the slurry. After the piston cap 16 has been inserted into the upper end of the backed column 10.

Automatically stops due to balance with the compacted filling material.Next, after releasing the clamp 92, the small jack 84
The rod 84a is retracted and activated, and the packing column 80 is pulled upward. After that, if necessary, tighten the screw 48 or port 58 of the piston-like cap 16, and attach the rear end body 20 of the piston-like cap 16 to the back column l.
After being locked to the inner wall surface of the main jack 88, the rod 88a of the main jack 88 can be retracted. As a result, a back column filled with a filler can be obtained.

The back column obtained by the apparatus shown in Fig. 8 also
Since the filling pressure has never been released after being pressed by the main jack 88, the high filling pressure is maintained.

In addition, in the apparatus shown in FIG. 8, if the fixed flange 68 is configured to be split into two, after pulling up the rod 88a, it is possible to take out only the backed column 10 and use it for chromatographic operation.

In the embodiment described above, a piston-shaped cap 16 is inserted into one end of the backed column 10, and the piston-shaped cap 16 is locked to the inner wall surface of the one end. Therefore,
A load is applied to the one end side of the backed column 10 in the direction of diameter expansion. To deal with this, it is extremely effective to increase the wall thickness of the one end of the parked column 10 or to wrap a reinforcing ring around the one end.

Although the rear end body 2° of the piston-like cap 16 described above is fixed to the inner wall surface of the backed column 10, the rear end body 20 may be fixed to the flange 10a of the backed column 10. In this case, a flange having approximately the same diameter as the flange 10a of the backed column 10 is integrally provided at the end of the rear end body 20 opposite to the tip body 18 side, and the flanges are fixed together by clamping or bolting. Fix by means.

In addition, when the piston-shaped cap is configured in this way, the present applicant has disclosed Japanese Patent Application No. 136594/1986 or
A backed column was made in advance at high pressure and high density using the method proposed in 0617.

The above-mentioned piston-shaped cap is attached to this column.

The back column 10 packed with the packing material at high pressure as described above is used for chromatographic separation operation, but during this separation operation or during its preparation, the packing pressure of the packing material A in the back column 10 may be lowered. If the filling condition decreases or the filling state becomes uneven, as shown in FIG.
is connected, and hydraulic pressure is introduced through the hydraulic pressure introduction hole 36.

Then, the plunger-shaped convex portion 26 is pressed by this oil pressure, and the tip body 18 is pushed in a direction away from the rear end body 20 and projected. This makes it possible to increase the filling pressure of the packing material A in the back column 10 and restore the uniform filling state.

Note that the amount of protrusion of the tip body 18 from the rear end body 20 does not require a very long distance.This is because it presses the filling material that has already been compacted.Normally, the stroke amount of the tip body is , about 5 to 10% of the total length of the backed column is sufficient. Moreover, for that reason, as the hydraulic pump 98,
A small capacity device such as a manual pump is sufficient.

In the present invention, as shown in FIG. 10, seven cumulators 100 may be connected to the pipe 96.
Ejection pressure can be applied to the tip body 18 without frequently operating the hydraulic pump.

Furthermore, in the present invention, as shown in FIG. 11, only the accumulator 102 holding high-pressure hydraulic oil may be connected to apply protrusion pressure to the tip body 18.

In the above embodiment, the plunger-shaped convex portion 26 is provided on the tip body L8.
is provided, and the cylindrical recess 34 is provided in the rear end body 2o, but conversely, the cylindrical recess 34 may be provided in the tip body 18, and the plunger-shaped convex portion 26 may be provided in the rear end body 2o.
The working pressure medium is.

In addition to oil, other liquids such as water may be used, or compressed gas may be used.

[Effect of the Invention J] As is clear from the above description, according to the apparatus of the present invention, it is possible to repressurize the packing material that has already been compacted and packed in the back column. Therefore, when the filling pressure of the packing material decreases or the filling state becomes uneven during chromatography separation operation or preparation, it is necessary to repressurize to restore the filling pressure and restore or maintain a uniform filling state. It is considered a rotation.

Furthermore, according to the apparatus of the present invention, a backed column can be obtained without releasing the pressure for a long time after the completion of the high-pressure filling operation, so a backed column can be obtained in which the high-pressure filling effect is maintained. In addition, it is possible to take out only the backed column, and it is also possible to obtain a large number of backed columns with one device. Therefore, it is possible to simplify or downsize the structure of the chromatography apparatus and to reduce the cost of the structure of the chromatography apparatus.

[Brief explanation of drawings]

FIG. 1 is a vertical sectional view showing an embodiment of the device of the present invention, FIG.
3 and 5 are longitudinal sectional views of the piston-shaped cap, FIG. 4 is a perspective view of the main part of FIG. 3, and FIG. 6 is a sectional view taken along the line 1--2 of FIG. 5. Figures 7 and 8 are cross-sectional views illustrating the method of filling the packed column with packing material; Figure 9;
FIGS. 1O and 11 are cross-sectional views illustrating the protruding operation of the tip body. lO...Backed column, 12...Perforated plate, 14.
... Cap, 16... Piston-shaped cap, 18... Tip body, 20... Rear end body, 80...
...Filling column. Agent Patent Attorney Shigeno
Figure 1 Figure 3 Figure 4 Figure 6 Figure 8

Claims (3)

[Claims] (1) In a chromatography apparatus having a chromatography column closed at both ends with a cap having a perforated plate through which a fluid can pass, and in which the column is filled with a packing material, the cap on one end side is It is capable of sliding inside the chromatography column, and is divided into a tip body on the front end side in the column insertion direction and a rear end body on the rear end side, and this rear body is connected to the chromatography column on the one end side. What is claimed is: 1. A chromatography apparatus, characterized in that the chromatography apparatus is capable of being stopped, and is provided with a pressing means for causing the leading end body to protrude from the trailing end body. (2) The locking of the rear end body to the chromatography column is as follows:
2. The chromatography apparatus according to claim 1, wherein the rear end body is pressed against and locked onto the inner wall surface of the chromatography column by protruding a side circumferential surface of the rear end body. (3) The pressing means includes a cylindrical recess provided on one of the facing surfaces of the tip end body and the rear end body, a plunger-like protrusion provided on the other of the facing surfaces and fitted into the recess, and The chromatography apparatus according to claim 1 or 2, characterized in that the rear end body includes a through hole for a working medium for pressing the plunger-shaped convex portion.