JPH0375068B2 - - Google Patents

Description

[Detailed Description of the Invention] [Industrial Application Field] The present invention relates to a chromatography device such as liquid chromatography, glass chromatography, or supercritical chromatography, and particularly relates to a chromatography device packed in a chromatography column. This is a chromatography device that can repressurize the packed material.

[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 device uses a chromatography column filled with a packing material of microparticle size, and the packing material must be packed in this chromatography column with high density and uniformity. This makes it possible to exhibit superior separation performance. Conventionally, in order to fill a chromatography e-column with a packing material at high pressure, the method used was to connect a packing device (for example, a high-pressure pump) to the chromatography e-column, perform high-pressure filling, and then attach a removal stopper to the filling device after filling. It is being said.

A method is also known in which a piston is inserted into a chromatography column and the slurry of the packing material introduced into the column is concentrated 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 filler material decreases or the filling state becomes uneven, it is difficult to take prompt action. 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 bridging phenomenon of the packing material, but as the diameter increases,
The degree of release of the filling pressure when the filling device is removed increases, and the effect of high-pressure filling becomes smaller.

In addition, when inserting a piston into a chromatography column and filling it under high pressure, as in Japanese Patent Publication No. 58-20284, it is possible to pressurize the packing material again.
It is also possible to maintain the effects of high pressure filling. 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 that is closed at both ends with a cap having a perforated plate through which a fluid can pass. In the case where the cap is filled with a filler material, the cap at one end is shaped like a piston and is divided into a tip end and a rear end. A locking means is provided to lock the rear end body to the chromatography column. As this locking means, a member is used which can be locked to the inner wall surface of the chromatography column by protruding a member from the side peripheral surface of the rear end body and pressing it against the inner wall surface of the column. Further, a pressing means for advancing the distal end body in the insertion direction from the rear end body is provided. Hereinafter, the column filled with this packing material will be referred to as a packed column, and the cap that slides inside the packed column will be referred to as a piston-shaped cap.

[Function] In the chromatography apparatus of the present invention,
By causing the leading end to protrude from the trailing end, it is possible to repressurize the packing material already packed in the packed column under high pressure.

Furthermore, in the chromatography apparatus of the present invention,
Introducing the packing material slurry into the packed column,
This can be pressed by the piston-like cap, and then the projectable member on the side circumferential surface of the rear end of the piston-like cap can be made to protrude and be locked to the inner wall surface of the packed column as it is. Therefore, according to the present invention:
It is possible to maintain the pressure at the time of filling the packed column.

Further, after filling, the packed column can be separated from an attached packing device, such as a piston-like cap pushing device, so that the structure 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, reference numeral 10 denotes a packed column loaded with packing material, A
is the packing material layer packed in this column. One end of this packed column 10 (upper end in the figure)
A cap 14 having a perforated plate 12 is attached thereto. Note that the perforated plate 12 is made of a material such as sintered metal or porous ceramics that allows only liquid or gaseous fluid to pass therethrough and does not allow the filler to pass therethrough. In this embodiment, the cap 14 is connected to the upper end of the packed column 10 by a clamp 15, but the packed 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 packed column 10 (lower end in the figure).

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

The piston-like cap 16a shown in FIG. 2 is divided into a leading end 18 and a trailing end 20. As shown in FIG. Second
In the posture shown in the figure, the upper surface of the tip body 18 is shallowly gouged to form a recess 22, and the perforated plate 12 is fixed so as to cover the recess 22. Moreover, this recess 22 is connected to the piston-shaped cap 1.
A communication hole 24 for communicating with the opposite side of 6a is
It is perforated in the axial direction of the tip body 18. A thick cylindrical plunger-like convex portion 26 is bored on the lower surface side of the tip body 18 in the drawing. Further, a seal ring 28 is wound around the side peripheral surface of the tip body 18, and this seal ring is fixed by a scraper portion 30 that is a part of the seal ring and a nut 32 that is screwed onto the tip body 18. has been done.

On the other hand, the rear end body 20 has a cylindrical recess 3 having a circumferential groove shape into which the plunger-like convex portion 26 is inserted.
4 is drilled. These convex portions 26 and concave portions 3
4, hydraulic pressure can be introduced from a hydraulic pressure introduction hole 36 provided in the rear end body 20. code 38
O-rings a and 38b perform hydraulic sealing.

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

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

The cap fixing tapered rings 42, 44 have slopes 42a, 44a that slide against each other,
By pushing the taper ring 44 upward in the figure, the taper ring 42 bulges out, and it is possible to lock the rear end body 20 to the inner wall surface of the packed column 10. In this example of FIG.
is screwed onto the rear end body 20 by inserting the presser ring 46, and when this screw 48 is tightened, the taper ring 44 is inserted by the taper ring presser ring 46.
is pushed and moved so as to sneak into the inside of the taper ring 42, and the taper ring 42 can bulge out from the side circumferential surface of the rear end body 20.

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 that is smaller in height on the inner circumferential side than on the outer circumferential side, and is arranged on the outer circumferential side of the tapered ring 50 at a predetermined distance. 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 angle of inclination that allows sliding. ing.

A bolt 58 is inserted through the taper ring 56, and the tip of the bolt 58 is inserted into the taper ring 54.
It is screwed on. Therefore, when the bolt 58 is tightened, the taper rings 54, 56 are moved in the approaching direction, and thereby the taper ring 52 bulges out from the side surface of the rear end body 20b.

Piston-shaped cap 1 shown in FIGS. 5 and 6
6c, four contact members 60 are provided. As shown in FIG. 6, which is a sectional view taken along the line in FIG. is attached to. Further, the outer circumferential surface of the contact member 60 is made of, for example, hard rubber, which has a large frictional resistance. Furthermore,
The arm 64 has both ends connected to the abutting member 60 and the rear end body 2.
It is pivotally supported by 0. This arm 64 is inclined upward toward the center of the rear end body 20 in the illustrated attitude. When the piston-shaped cap 16c is moved upward in the figure, the arm 64 receives a force that causes it to rotate in the direction of the arrow θ, thereby reducing the frictional force between the contact member 60 and the packed column 10 or the inner circumferential surface of the packing column to be described later. The weak, piston-like cap 16c can slide smoothly inside the packed column 10 or packing column. on the other hand,
When the piston-like 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 packed column 10 or the packing column increases, and the piston-shaped cap 16c is locked 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 short, the rear end body 20 of the piston-shaped cap 16 may have any structure as long as it can be securely engaged with the packed column 10, and may have a structure other than that shown in FIGS. 2 to 6. good.

Next, with reference to FIGS. 7 and 8, an example of a method for filling the packed column 10 with a filler under high pressure will be described.

In FIG. 7, the packed column 10 is erected on a packing device 66. packed column 1
A flange 10a is provided at the lower end of 0, and this flange 10a is connected to a fixed flange 68 with a clamp 70. Fixed flange 68
is fixed to a support base 74 via a fixing 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 packed column 10, and the packed column 10 is installed coaxially with the through hole 78.

A packing column 80 having an inner diameter approximately equal to that of the packed column 10 is installed between the support base 74 and the fixed flange 68. This packing column 80 is connected to a mounting base 82, and this mounting base 82 is moved up and down by a small jack 84. The small jack 84 is fixed to the support base 74, and the piston rod 84
a 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 detachably connected to the fixed flange 68 by a clamp 86. Note that the packing column 80 is located coaxially with the packed column 10.

Reference numeral 88 is a main jack fixed to the support base 74, and a piston rod 88a of this main jack 88 moves the piston-shaped cap 16 from the lower end of the packing column 80 to the packed column 1.
It has a stroke amount that allows pressing movement to the lower end insertion position of 0.

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

First, pull in the rod 88a of the main jack 8,
The filling column 80 is retracted to below the lower end, and the piston-shaped cap 16 with the seal ring 28 adjusted is inserted from the bottom of the filling column 80.
It is supported by a rod 88a.

After that, the clamp 15 is released and the cap 14 is closed.
is removed from the upper end of the packed column 10, and the slurry liquid of the packing material is injected into the packed column 10 and the packing column 80. After injection of a predetermined amount is completed, the cap 14 is placed over the packed column 10,
Fix with clamp 15. And the main jack 8
8 to protrude the rod 88a and gradually move the piston-like cap 16 upward. Note that the rear end body 20 of the piston-shaped cap 16
The communication hole 40 is closed with a blind plug (not shown) to prevent the liquid in the slurry from leaking out from the piston-shaped cap 16 when the slurry is injected and when the piston-shaped cap 16 is raised. It's summery.

The piston-shaped cap 16 is further pressed upward,
Insert into the lower end of the packed column 10. and,
The pressure of the compacted filler and 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,
The packing column 80 is gradually moved downward.

After that, if the piston-like cap 16 has the configuration 16a or 16b shown in FIG. urge (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, the packed column 10 filled with the filler material is obtained. be able to.

Packed column 10 obtained in this way
The pressure charged by the main jack 88 is 1
Since the pressure is maintained without being released, a uniform high-pressure filling state is maintained.

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. 8, packed column 1
0 is supported by the inner periphery of the through hole 78 of the fixed flange 68 via the stop member 90. The flange 10a of the packed column 10 and the flange 80a of the packing column are removably connected by a clamp 92.

Note that in the device shown in FIG. 8, the leg portion 76 is omitted;
Instead, a fixed base 94 is installed, and the packed column 10 is erected on the fixed base 94. Furthermore, the fixed rod 72 is attached to this fixed base 94.
and a support base 74, and the distance therebetween is maintained constant. 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-like 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 operated to pull it out to the outside of the packing column 80. Next, the slurry liquid of the packing material is injected into the packed column 10 and the packing column 80 from the upper part of the packed column 80. After injecting a predetermined amount of the filler slurry liquid, the piston-shaped cap 16 with the adjusted seal ring 28 is inserted into the filling column 80, and the rod 88a of the main jack 88 is caused to protrude. The piston-like cap 16 is then moved downward, inserted into the packed column 80, and gradually pushed further downward. This pressing down gradually consolidates the slurry. Piston-shaped cap 16
is inserted into the upper end of the packed column 10,
Automatically stops due to balance with compacted filling material. Next, after releasing the clamp 92, the rod 84a of the small jack 84 is retracted and activated.
The packing column 80 is pulled upward. After that,
If necessary, the screw 4 of the piston-like cap 16
8 or the bolt 58 to lock the rear end body 20 of the piston-like cap 16 to the inner wall surface of the packed column 10, then tighten the rod 8 of the main jack 88.
8a can be retracted. Thereby, a packed column filled with the filler can be obtained.

The packed column obtained by the apparatus shown in FIG. 8 also maintains a high packing pressure since the packing pressure has never been released after being pressed by the main jack 88.

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 packed column 10 and use it for chromatographic operation.

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

The rear end body 20 of the piston-like cap 16 described above
2 shows an example in which the rear end body 20 is fixed to the inner wall surface of the packed column 10.
It may be fixed to the flange 10a of 0. In this case, a flange 10a of the packed column 10 is provided at the end of the rear end body 20 opposite to the lost body 18 side.
A flange with approximately the same diameter is provided integrally. Then, the flanges are fixed together using fixing means such as clamps or bolts.

It should be noted that when the piston-shaped cap is configured in this way, the present applicant has proposed patent application No. 60-136594 (Japanese Unexamined Patent Publication No.
61-294361) or 150617 (JP-A-62-
A packed column with high pressure and high density is made in advance using the method proposed in 11161), and the above-mentioned piston-shaped cap is attached to this column.

The packed column 10 filled with the packing material under high pressure as described above is used for chromatographic separation operation, but during this separation operation or during its preparation, the packing material A in the packed column 10 is
If the filling pressure decreases or the filling state becomes uneven, as shown in FIG. Introduce hydraulic pressure through. Then, due to this hydraulic pressure, the plunger-shaped convex portion 2
6 is pressed, and the tip end 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 packed column 10 and restore the uniform filling state.

Note that the amount of protrusion of the distal end body 18 from the rear end body 20 does not require a very long distance. This is to press the filling material that has already been compacted. Usually, a stroke amount of the tip body of about 5 to 10% of the total length of the packed column is sufficient. Further, for this reason, a small-capacity hydraulic pump such as a manual pump is sufficient as the hydraulic pump 98.

In the present invention, as shown in FIG.
The accumulator 100 may be connected to. In this way, protrusion pressure can be applied to the tip body 18 without frequently operating the hydraulic pump.

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

In the above embodiment, the plunger-like convex portion 26 is provided on the tip body 18, and the cylindrical recess 3 is provided on the rear end body 20.
4, however, conversely, the cylindrical recess 34 may be provided on the tip end 18 and the plunger-like protrusion 26 may be provided on the rear end 20. Further, the working pressure medium may be other liquids such as water in addition to oil. Compressed gas may also be used.

[Effects of the Invention] 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 packed column. Therefore, when the filling pressure of the packing material decreases or the filling state becomes uneven during chromatographic 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 possible.

Furthermore, according to the apparatus of the present invention, a packed column can be obtained without releasing the pressure for a long time after the completion of the high-pressure filling operation, so a packed column can be obtained in which the high-pressure filling effect is maintained. In addition, it is possible to take out only the packed column, and 1
It is possible to obtain a large number of packed columns with one apparatus. Therefore, it is possible to simplify or downsize the configuration of the chromatography device and to reduce the cost of constructing the chromatography device.

[Brief explanation of drawings]

FIG. 1 is a longitudinal sectional view showing an embodiment of the device of the present invention;
Figures 2, 3, and 5 are longitudinal sectional views of the piston-like cap, Figure 4 is a perspective view of the main part of Figure 3, and Figure 6 is a perspective view of the main part of Figure 3.
The figure is a sectional view taken along the - line in FIG. 5. 7th
8 and 8 are sectional views illustrating the method of filling the packed column with filler, and FIGS. 9, 10, and 11 are sectional views illustrating the protruding operation of the tip body. 10...Packed column, 12...Perforated plate, 14...
Cap, 16... Piston-shaped cap, 18... Tip body, 20... Rear end body, 80... Filling column.

Claims (1)

[Scope of Claims] 1. 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 one end comprising: The side cap is a piston-shaped cap that can slide 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. has a member that can protrude from its side peripheral surface, and can be locked to the chromatography column at one end by pressing the member against the inner wall surface of the column, and the tip body is connected to the rear end body. A chromatography apparatus characterized in that it is provided with a pressing means for moving the device forward in the insertion direction. 2. The pressing means includes a cylindrical recess provided on one of the facing surfaces of the tip body and the rear end body, a plunger-like convex portion provided on the other of the facing surfaces and fitted into the recess, and the rear end body. The chromatography apparatus according to claim 1, characterized in that the end body includes a through hole for a working medium for pressing the plunger-like convex portion, which is formed in the end body.