JPS6242052A - Chromatography device - Google Patents

Abstract

PURPOSE:To recover filling pressure of a packed column by setting the cap of a chromatography column at one end side in a slidable piston-like shape and providing a cap pressurizing device pressing and moving in the column. CONSTITUTION:A cap 14 having a perforated panel 12 is loaded on one end of the packed column 10 where a filling material is filled, and is linked to the upper end of the column 10 with a clamp 15. A piston-like cap 16 is inserted on the other end of the column 10, and can be pressurized by a pressurizing device 18. The periphery side of the cap 16 is projecting, and accordingly the cap can be locked on the inner wall surface of the column 10. Thus the filling pressure of the column 10 can be recovered.

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 chromatography equipment such as liquid chromatography, gas chromatography, or supercritical chromatography. This invention relates to a chromatography device that can be pressurized.

[Prior Art] Liquid chromatography and gas chromatography are known as devices for separating specific components from a solution or mixed gas. As is well known, this chromatography device uses a chromatography column filled with a packing material of microparticle size, and by packing the packing material in the chromatography column with high density and uniformity, excellent performance can be achieved. Separation performance can be demonstrated. Conventionally, in order to fill the filler material into the chromatographic dam at high pressure,
A method is used in which a filling device (for example, a high-pressure pump) is connected to a chromatography column, high-pressure packing is performed, and a removal stopper is attached to the pre-filling device after filling.

Another method is known in which a piston is inserted into a chromatography column, and the piston condenses and compacts the slurry of the packing material introduced into the column.
8-20284).

[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, for example, the packing material becomes loose or the filling state becomes uneven during the chromatography operation, it is difficult to take prompt action.

Furthermore, since the stopper is once removed, the filling pressure is released for a long period of time, which tends to reduce the effect of repressurization.

In addition, as in Japanese Patent Publication No. 58-20284, when inserting a piston into a chromatographic column and filling it with high pressure, it is possible to pressurize again by leaving the piston in the chromatographic column as it is; Since the column and the large 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 cap at both ends having a perforated plate through which liquid can pass, or has a chromatography column, in which a packing material is placed. In the loaded device, the cap on one end side is a piston-shaped cap that can slide inside the chromatography column, and a cap pressing device is provided to press and move the piston-shaped cap.

Note that, hereinafter, a column loaded with this packing material will be referred to as a backed column.

[Function] In the device of the present invention, the filling pressure can be increased or restored by pushing the piston-shaped cap in the back column filled with filler into the back column using a pressing device.

[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.

Reference numeral 10 is a backed column loaded with a packing material.

A cap 14 having a perforated plate 12 is attached to one end (the upper end in the figure) of this perforated column 10. Note that the porous plate 12 is made of a material such as sintered metal or porous ceramics that allows only fluid (liquid or gas) to pass therethrough and does not allow the filler to pass through. In this embodiment, the cap 14 is connected to the upper end of the back column lO with a clamp 15;
It is also possible to provide flanges on both the cap 14 and the cap 14, and to connect them by tightening bolts.

A piston-shaped cap 16 is inserted into the other end of the backed column (lower end in the figure), and can be pressed by a pressing device 18.

This piston-shaped cap 16 has a structure that can be engaged with the inner wall surface of the backed column 10 by protruding its side peripheral surface. 16 configuration examples will be explained.

The piston-shaped cap 16a shown in FIG. 2 has a disc-shaped cap body 20. In the attitude shown in FIG.
2 are formed, and a perforated plate 12 is fixed so as to cover these four parts 22. Further, a communication hole 24 for communicating the four parts 22 with the opposite side of the piston-shaped cap 16a is bored in the axial direction of the cap body 20, and a curved recess 26 is formed at the lower end side opening of the communication hole 24. is formed. On the side peripheral surface of the cap body 20, from the top in the figure, a seal ring 28 and a seal retainer ring 30 are installed.
, a cap fixing taber ring 32, 34, and a taber ring holding ring 36 are attached.

The seal ring 28 has a side peripheral surface that is similar to the backed column 10.
It also slides against the inner circumferential surface of a packing column, which will be described later, to achieve a seal. The seal retainer ring 30 is attached to the cap body 2
The cap body 20 is attached to the cap body 20 by a bolt 38 screwed into the cap body 20, and the bolt 38 is tightened to expand the seal ring 28 and seal the cap body 20 and the backed column 10.

The cap fixing taber rings 32 and 34 have slopes 32a and 34a that slide against each other.
4 upward in the figure, the taper ring 32 bulges out, and it is possible to lock the piston-shaped cap 16a to the inner wall surface of the backed column 10. This second
In the illustrated example, a screw 40 is inserted through a presser ring 36 and is screwed onto the seal presser ring 30. When the screw 40 is tightened, the tapered ring presser ring 36 approaches the seal presser ring 30 side. As a result, the taper ring 34 is pressed and moved so as to sneak inside the taper ring 32, and the taper ring 32 is pushed into the piston-like cap 16.
It can bulge out from the side peripheral surface of a.

In the piston-like cap 16b of FIG. 3, tapered rings 42, 44 are used.

As shown in FIG. 4, the tapered ring 42 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 fixed to the cap body 20. On the other hand, the tapered ring 44 is a ring having a trapezoidal cross-section with a height smaller on the inner side than on the outer side, and is arranged on the outer side of the tapered ring 42 at a predetermined distance.

As shown in FIG. 3, further different taper rings 46 and 48 are J-shaped so as to sandwich these taper rings 42 and 44, and the slopes of each taper ring 42 to 48 have an inclination angle at which they can slide. It is said that

A bolt 50 is inserted through the taper ring 48, and the tip of this bolt h50 is screwed into the taper ring 46. Therefore, when the bolt 50 is tightened, the taper ring 56.
58 is moved in the proximal direction vi, thereby causing the taper ring 44 to bulge out and close the piston-shaped cap 36.
protrudes from the side of b.

In the piston-shaped cap 16c shown in FIGS. 5 and 6, four contact members 52 are provided. The contact member 52 is shown in FIG.
As shown in the figure, it is a piece-like member having an outer peripheral surface curved into an arc shape, and is attached to the cap body 20 via a spring 54. Further, the outer circumferential surface of the contact member 52 is made of a material with high frictional resistance, such as hard rubber. Furthermore, the arm 56 is pivotally supported at both ends by the abutment member 52 and the cap body 20. This arm 56 is inclined upward toward the center of the cap body 20 in the illustrated attitude. When this piston-shaped cap 16c is moved upward in the figure, the arm 56 receives the force of rotation in the direction of arrow 0, and the frictional force between the contact member 52 and the back column 10 or the inner circumferential surface of the packing column to be described later is reduced. Weak, piston-shaped cap 16c
can slide smoothly inside the back column 10 or the first packed column. On the other hand, when the piston-shaped cap 16c receives a downward force in the figure, the arm 56 rotates in the counter-θ direction, the frictional force between the contact member 52 and the inner peripheral surface of the back column 10 or the packing column increases, and the piston A shaped cap 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 Z6a, so the same members are given the same reference numerals and their explanations will be omitted.

In short, the piston-shaped cap 16 may have any structure as long as it can securely lock onto the inner circumferential surface of the backed column IO, and may have a structure other than that shown in FIGS. 2 to 6. .

Next, the configuration of the pressing device 18 shown in FIG. 1 will be explained.

A flange-shaped upper plate 58 is attached to the lower end of the backed column IO via a clamp 60, and this upper plate 58 is connected to a lower plate 64 via a connecting rod 62. This lower plate 64 is
It is fixed to a jack 66, and the jack 66 is erected by a suitable support member (not shown).

The jack 66 is equipped with a rod 66a that can protrude upward, and by pushing the piston-shaped cap 16 with this rod 66a, the packing material A in the back column 10 is removed.
By increasing the filling pressure of the filling material A, loosening and non-uniformity of the filling material A can be eliminated.

Note that since this jack 66 is used to press the filling material that has already been filled with high pressure, its stroke amount may be small.

(For example, if the total length of the backed column is 1 m, a stroke amount of about 100 mm is sufficient.) Jacket 6
A specific example of the rod 66a is one in which the rod 66a is a male screw, and a nut is provided on the main body side to be screwed with the male screw f-, and the rod 66a is made to appear and retract by rotating the nut. It will be done.

Next, an example of a method of filling force of the packing material into the backed column 10 shown in Fig. m1 will be explained with reference to Fig. 7.

In FIG. 7, the flange 10a at the lower end of the backed column 10 is connected to the fixed flange 68 by a clamp 70. The 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 water H7° attitude.

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 10, and the backed column 10 is installed coaxially with this through hole 58.

Between the support base 74 and the fixed flange 68 is a packing column 8 having an inner diameter approximately equal to that of the backed column IO.
0 is set. 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 its piston rod 84a extends to one side, 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 backed column 10.

Reference numeral 88 denotes 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 10. It has a stroke amount that can be used.

Next, a procedure for filling the filler using the apparatus shown in FIG. 7 will be described.

First, loosen the taper ring 34 and remove the piston-shaped cap 1.
6 can move freely, main jack 88
The piston-shaped cap 16 is inserted under the packing column 80 and supported by the rod 88a, as shown by the two-dot chain line in FIG.

Thereafter, the clamp 15 is released, the cap 14 is removed from the upper end of the backed column 10, and the slurry of the packing material is injected into the backed column 10 and the packing column 80. After the injection of the predetermined gate is completed, the cap 14 is placed on the back column IO and fixed with the clamp 15. and,
The main jack 88 is actuated to project its rod 88a and gradually move the piston-like cap 86 upward. Note that the communication hole 24 of the piston-shaped cap 86 is closed with a blind plug (not shown), so that when the slurry is injected and the piston-shaped cap 16.4 is operated in one direction, the liquid in the slurry flows into the piston-shaped cap 16. It will not leak out.

The piston-like cap 16 is further pushed up and inserted into the lower end of the backed column 10.

Next, after releasing the clamp 86, the small jack 84 is operated to retract the opening 7 door 84a, and the filling column 8 is opened.
0 gradually downward.

After this, if the piston-like cap 16 has the configuration 16a or 16b shown in FIG. 2 or 3, the screw 40
Or, tighten the port 50 and remove the piston-shaped cap 16b.
Alternatively, 16c is locked 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.

In this manner, the obtained backed column 10 maintains the high pressure filled by the main jack 88 without ever releasing it, and thus maintains a uniform high pressure filled state.

FIG. 8 is a longitudinal cross-sectional view showing a different method of filling the back column 10, and the embodiment shown in FIG. 8 has a structure in which the structure shown in FIG. 7 is turned upside down.

In the apparatus shown in FIG.
is supported on the inner circumference of the The flange 10a 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 curved recess 26 of the piston-shaped cap 16 (see FIGS. 2 to 5).

The rest of the configuration of the device in FIG. 8 is the same as that in FIG. 1 except that the device is turned upside down, so the same reference numerals are given to the same members and the explanation thereof will be omitted.

Next, the procedure for loading the filler in the apparatus shown in FIG. 8 will be explained.

First, the rod 88a of the main jack 88 is retracted and operated, and then the slurry liquid of the packing material is injected into the back column IO and the packing column 80 from the upper part of the packing column 80. After injecting a predetermined amount of the filler slurry liquid, the piston-shaped cap 16 is inserted into the filling column 80, the rod 88a of the main jack 88 is made to protrude, and the piston-shaped cap 1
6 is moved downward, inserted into the packed column 80, and further pushed down gradually. This pressing down gradually consolidates the slurry. After the piston-like cap 16 is inserted into the upper end of the backed column 1o, the main jack 88
Then, after releasing the clamp 92, the rod 84a of the small jack 84 is retracted and activated to pull the filling column 8o downward. After that, if necessary,
Tighten the screw 40 or port 5o of the piston-shaped cap 16, and attach the piston-shaped cap 16 to the back column 10.
After being locked to the inner wall surface of the main jack 88, the load 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.

When performing chromatographic operations on a back column packed with packing material under high pressure in this way, or during preparation, if the packing pressure in the back column decreases or the packing state becomes uneven, it is necessary to As shown in FIG. 1, the backed column 10 is connected to a pressing device fi 18.

Then, the rod 66a of the jack 66 is pressed against the piston-shaped camp 16. (The piston-shaped cap 16.

Those with the configuration shown in Figure 2 or Figure 3 (16a, 16b)
If so, loosen Porto 4o or 5o at this point. ) Next, push the piston-shaped cap into the back column O with strong pressure using the rod Baa, and fill the packing material A.
Increase the filling pressure.

Next, the piston-like cap 16
In the case of 16a or 16b in the figure, tighten the screw 40 or bolt 50 to fix the piston-shaped cap 16. (It can be moved and locked without loosening or tightening.) In the filling device shown in Figs. In this case, it is better not to make the slurry concentration too high, or to use a somewhat longer backed column.

In this manner, the apparatus of the present invention can further press the packing material A that has already been packed at high pressure into the backed column 10, thereby recovering the filling pressure and eliminating the uneven packing state.

In the apparatus of the embodiment shown in FIG. 1, a piston-shaped cap 16 that can be locked to the inner wall surface of the back column is inserted at the lower end in the figure, and when trying to press the filler A, this piston-shaped cap with a locking function is inserted. I try to push it in, but
In the present invention, as shown in FIG. 9, a piston-shaped cap 96 without a locking function may be inserted. In this case, it is necessary to keep the piston-shaped cap 96 pressed at all times, so that the back column 10 and The pressing device is integrated during chromatographic separation operations.

Further, in order to first fill the packed column with the packing material, it may be carried out using a conventional filling device such as a high-pressure pump, or by the method disclosed in Japanese Patent Publication No. 58-20284.

In addition, in FIG. 9, a recess 96b is formed on the upper surface of the cap body 96a, and the perforated plate 12 is attached thereto.
It communicates with the lower surface through a communication hole 96c. 96d is a seal ring, which is fastened by a retainer ring 96e that is threadedly engaged with the gap body 96a. 96f is a curved portion that engages with the tip of the jack rod 88a.

When the piston-shaped cap shown in FIGS. 2 to 6 is used, the piston-shaped cap 16 is inserted into one end of the backed column 10 as diagonally above, and the side circumference of this piston-shaped cap 16 is attached to the inner wall surface of the one end. The surface protrudes and is locked. Therefore, a load is applied to the one end side of the back column IO in the direction of diameter expansion. To deal with this, it is extremely effective to increase the thickness of the one end of the backed column IO or to wrap a reinforcing ring around the one end.

In the above description, the backed column 10 is installed vertically, but the pack 1 column 10 may be installed diagonally or horizontally.

[Effects of the Invention] As is clear from the above description, according to the apparatus of the present invention, even the packing material already packed at high pressure in the backed column can be re-pressurized without frequently releasing the packing pressure. , it is possible to restore the filling pressure, eliminate non-uniformity, etc. Furthermore, it is also possible to simplify or downsize the configuration of the chromatography device, thereby reducing the cost of constructing the chromatography device.

[Brief explanation of the drawing]

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 Vl-V of FIG. 5.
It is a sectional view along I line. 7 and 8 are cross-sectional views illustrating the procedure for loading the packing material into the backed column 10. FIG. FIG. 9 is a cross-sectional view of the piston-like cap 96. DESCRIPTION OF SYMBOLS 10... Backed column, 12... Perforated plate, 14... Cap, 16... Piston-shaped cap, 66... Pressing device. Agent Patent Attorney Tsuyoshi Shigeno Figure 2 Figure 3'su bu Figure 5 Figure 6

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, one end side of the chromatography column is provided. The cap is
A chromatography apparatus comprising a piston-shaped cap that is slidable within the chromatography column, and a cap pressing device that presses and moves the piston-shaped cap within the chromatography column. (2) The chromatography apparatus according to claim 1, wherein the piston-shaped cap can be locked to the inner wall surface of the chromatography column by protruding a side peripheral surface thereof. (3) Claim 1, characterized in that the cap pressing device is provided integrally with the chromatography column.
The chromatography device described in Section.