JPH0375066B2 - - Google Patents

Description

Detailed Description of the Invention [Industrial Application Field] The present invention relates to chromatography equipment such as liquid chromatography, gas chromatography, or supercritical chromatography, and particularly relates to chromatography equipment such as liquid chromatography, gas chromatography, or supercritical chromatography, and in particular, to This invention relates to a chromatography device that can be filled without releasing the filling pressure.

[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, when attaching a stopper, it is necessary to remove the packing device from the chromatography column and then attach the stopper. Therefore, there is a problem that the filling pressure of the filling material is temporarily released.

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 before plugging, the effect of high-pressure packing will be small. Become. 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 packing pressure when the packing device is removed increases, resulting in high-pressure packing. effect becomes smaller.

In addition, when inserting a piston into a chromatography column to perform high-pressure packing as in Japanese Patent Publication No. 58-20284, it is possible to maintain the effect of high-pressure packing by leaving the piston in the chromatography column as it is. 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. A packing material is loaded into the chromatography column, and the packing column is detachably attached to one end of the chromatography column and has approximately the same internal diameter as the chromatography column, The cap is a piston-shaped member that is movable through the packing column and into one end of the chromatography column, and is capable of moving the chromatography column by protruding a projectable member provided on its side circumferential surface. The cap can be locked to the inner wall surface of the chromatography column, and is characterized by being equipped with a cap moving device that presses and moves the cap on one end side through the packed column and into one end of the chromatography column. shall be.

Hereinafter, the column loaded with this packing material will be referred to as a packed column, and the cap that is passed through the packed column and the packing column will be referred to as a piston-shaped cap.

[Function] In the chromatography apparatus of the present invention, in order to fill the packed column with the packing material, the piston-shaped cap is retracted outside the packed column, for example, into the packing column, and the necessary amount is filled inside the packed column and the packing column. Introducing the amount of filler slurry. After that, activate the cap moving device,
This slurry is pressed with a piston-shaped cap, and the filler is gradually pressed into the packed column. Once the piston-like cap has been pushed into one end of the packed column, the cap moving device is stopped. The piston-shaped cap has a protruding side circumferential surface and is engaged with an inner wall surface at one end of the packed column.

Therefore, according to the present invention, it is possible to maintain the pressure at the time of filling the packed column. Furthermore, after packing, the connection between the packed column and the packing column can be released and the packed column can be separated from the packing column, so it is possible to simplify the configuration of the chromatography apparatus during use. be. In addition, a short length of the packed column is sufficient.

[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 is a packed column loaded with a packing material. This packed column 10 is installed in the vertical direction, and the upper end has a cap 14 having a perforated plate 12.
is installed. In addition, as the perforated plate 12,
Materials such as sintered metal and porous ceramics that allow only fluid (gas or liquid) to pass through but not fillers are used. cap 14
In this embodiment, the cap 10 is connected to the upper end of the packed column 10 by a clamp 16, but the packed column 10 and the cap 14 may be provided with flanges and connected by bolts.

A flange 10 is attached to the lower end of the packed column 10.
a is provided, and this flange 10a is connected to the fixed flange 18 with a clamp 20.
The fixed flange 18 is fixed to a support base 24 via a fixed rod 22, and
is installed while maintaining a horizontal posture by means of legs 26. The fixed flange 18 is attached to the packed column 1
The packed column 10 is provided coaxially with the through hole 28, which has a diameter equal to or larger than the outer diameter of the column.

A packing column 30 having an inner diameter approximately equal to that of the packed column 10 is installed between the support base 24 and the fixed flange 18. This packing column 30 is connected to a mounting base 32, and this mounting base 32 is moved up and down by a small jack 34. The small jack 34 is fixed to the support base 24, and its piston rod 34
a extends upward, and its tip is fixed to the lower surface of the mounting base 32.

A flange 30a is provided at the upper end of the packing column 30, and this flange 30a is detachably connected to the fixed flange 18 by a clamp 35. Note that the packing column 30 is located coaxially with the packed column 10.

Reference numeral 36 indicates a piston-shaped cap, which can be inserted through the packing column 30 to the lower end portion of the packed column 10. Reference numeral 38 denotes a main jack fixed to the support base 24, and a piston rod 38a of the main jack 38 presses and moves the piston-shaped cap 36 from the lower end position of the packing column 30 to the lower end insertion position of the packed column 10. It has the amount of stroke you get.

The piston-shaped cap 36 has a structure in which it can be engaged with the inner wall surface of the packed column 10 by protruding its side peripheral surface.

Next, an example of the structure of the piston-shaped cap 36 will be explained with reference to FIGS. 2 to 5.

The piston-shaped cap 36a shown in FIG. 2 has a disk-shaped cap body 40. In the attitude shown in FIG. 2, the upper surface of the cap body 40 is shallowly hollowed out to form a recess 42, and the perforated plate 12 is fixed so as to cover the recess 42. Also, a communication hole 44 for communicating this recess 42 with the opposite side of the piston-shaped cap 36a.
is bored in the axial direction of the cap body 40, and the lower end opening of this communication hole 44 has a curved recess 4 on which the tip of the rod 38a of the main jack 38 is seated.
6 is formed. On the side peripheral surface of the cap body 40, from the top in the figure, a seal ring 48, a seal retaining ring 50, cap fixing tapered rings 52, 54, and a tapered ring retaining ring 56 are arranged.
is installed.

The seal ring 48 has a side circumferential surface that slides on the inner circumferential surface of the packed column 10 or the packing column 30 to perform sealing. Seal holding ring 50
is attached to the cap body 40 by a bolt 58 screwed into the cap body 40, and the bolt 58 is tightened to expand the seal ring 48 and seal the cap body 40 and the packed column 10.

The cap fixing tapered rings 52, 54 have slopes 52a, 54a that slide against each other,
By pushing the taper ring 54 upward in the figure, the taper ring 52 bulges out, making it possible to lock the piston-shaped cap 36a to the inner wall surface of the packed column 10. In the example shown in FIG. 2, the screw 60 is inserted through the presser ring 56 and is screwed onto the seal presser ring 50. When the screw 60 is tightened, the taper ring presser ring 56 is screwed into the seal presser ring 50.
6 approaches the seal retaining ring 50 side, and as a result, the taper ring 54 is pressed and moved so as to sneak inside the taper ring 52, and the taper ring 52
may bulge out from the side peripheral surface of the piston-like cap 36a.

In the piston-like cap 36b of FIG. 3, tapered rings 62, 64 are used.
As shown in FIG. 4, the tapered ring 62 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 40. On the other hand, the tapered ring 64 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 at a predetermined distance from the tapered ring 62. As shown in FIG.
Further different taper rings 66, 6 sandwiching 4
8 is installed, and each taper ring 62 to 68
The slopes of each have an inclination angle that allows sliding.

A bolt 70 is inserted through the taper ring 68, and the tip of the bolt 70 is connected to the taper ring 66.
It is screwed on. Therefore, when the bolt 70 is tightened, the taper rings 66, 68 are moved in the approaching direction, so that the taper ring 64 bulges out from the side surface of the piston-like cap 36b.

Piston-shaped cap 3 shown in FIGS. 5 and 6
6c, four contact members 72 are provided. As shown in FIG. 6, which is a sectional view taken along the line in FIG. installed. Further, the outer circumferential surface of the contact member 72 is made of a material with high frictional resistance, such as hard rubber. Further, an arm 76 is pivotally supported at both ends by the abutment member 72 and the cap body 40.
In the illustrated attitude, the arm 76 is inclined upward toward the center of the cap body 40. When this piston-shaped cap 36c is moved upward in the figure, the arm 76 receives the force of rotation in the direction of arrow θ, which weakens the frictional force between the contact member 72 and the inner peripheral surface of the packed column 10 or the packing column 30. , the piston-like cap 36c can slide smoothly within the column 10 or 30. On the other hand, when the piston-shaped cap 36c receives a downward force in the figure, the arm 76 rotates in the opposite θ direction, and the frictional force between the contact member 72 and the inner peripheral surface of the packed column 10 or the packing column 30 increases,
A piston-shaped cap 36c is locked to the inner peripheral surface.

The other configurations of the piston-shaped caps 36b and 36c are the same as that of the piston-shaped cap 36a, so the same reference numerals are given to the same members and the explanation thereof will be omitted.

In short, the piston-shaped cap 36 may have any structure as long as it can be reliably engaged with the inner circumferential surface of the packed column 10, and as shown in FIGS.
It may have a structure other than that shown in the figure.

Next, a procedure for loading the filler in the embodiment apparatus shown in FIG. 1 will be explained.

First, the rod 38a of the main jack 38 is retracted, and the piston-shaped cap 36 with the adjusted seal ring 48 is inserted under the packing column 30 to support the rod 38a (the position indicated by the two-dot chain line in Fig. 1). ).

After that, the clamp 16 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 30. After injection of a predetermined amount is completed, the cap 14 is placed over the packed column 10,
Fix with clamp 16. And the main jack 3
8 to project its rod 38a and gradually move the piston-like cap 36 upward. Note that the communication hole 44 of the piston-shaped cap 36
is closed with a blind plug (not shown), so that liquid in the slurry does not leak out from the piston-like cap 36 when the slurry is injected and when the piston-like cap 36 is raised.

The piston-shaped cap 36 is further pressed upward,
Insert into the lower end of the packed column 10.

Next, after releasing the clamp 35, operate the small jack 34 to retract the rod 34a,
The packing column 30 is gradually moved downward.

After that, if the piston-shaped cap 36 has the configuration 36a or 36b shown in FIG. Lock it. (If the piston-like cap 36 has the configuration shown in FIG. 5, such screw or bolt tightening work is not necessary.) Thereafter, by releasing the clamp 20, a packed column 10 filled with the filler material is obtained. be able to.

In this way, the obtained packed column 10
is the pressure filled with high pressure by the main jack 38, 1
Since the pressure is maintained without being released, a uniform high-pressure filling state is maintained.

FIG. 7 is a longitudinal sectional view showing the configuration of a chromatography apparatus according to a different embodiment of the present invention, and the embodiment of FIG. 7 has a configuration in which the embodiment apparatus of FIG. have.

In the apparatus shown in FIG. 7, packed column 1
0 is supported by the inner periphery of the through hole 28 of the fixed flange 18 via a stopper member 78. The flange 10a of the packed column 10 and the flange 30a of the packing column are removably connected by a clamp 80.

Note that in the device shown in FIG. 7, the leg portion 26 is omitted;
A fixed base 82 is installed in its place, and the packed column 10 is erected on the fixed base 28. Furthermore, the fixed rod 22 is attached to this fixed base 82.
and the support base 24 are connected to each other, and the distance therebetween is maintained constant. Further, the tip (lower end in the figure) of the rod 38a of the main jack 38 is in contact with a curved recess 46 (see FIGS. 2 to 5) of the piston-like cap 36.

The rest of the configuration of the device in FIG. 7 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 embodiment apparatus will be explained with reference to FIG.

First, the rod 38a of the main jack 38 is retracted and operated. Next, the slurry liquid of the packing material is injected into the packed column 10 and the packing column 30 from the top of the packed column 30. After injecting a predetermined amount of the filler slurry liquid, the piston-shaped cap 36 is placed on the upper end of the packing column, the rod 38a of the jack 38 is made to protrude, and the piston-shaped cap 36 is
6 downward and inserted into the packed column 30,
Gradually press down further. This pressing down gradually consolidates the slurry. After the piston cap 36 has been inserted into the upper end of the packed column 10, the main jack 38 is stopped. Then,
After releasing the clamp 80, the rod 34a of the small jack 34 is retracted and operated, and the packing column 30 is
pull upwards. After that, the screw 60 or bolt 70 of the piston-like cap 36 is removed as necessary.
After tightening the piston-shaped cap 36 to the inner wall surface of the packed column 10, the rod 38a of the main jack 38 is retracted. This results in
A packed column filled with packing material can be obtained.

The packed column obtained by the apparatus shown in FIG. 7 also maintains a high packing pressure since the packing pressure has never been released after being pressed by the main jack 38.

In addition, in the apparatus shown in FIG. 7, if the fixed flange 18 is configured to be split into two, after pulling up the rod 38a, it is possible to take out only the packed column 10 and use it for chromatographic operation.

In the above embodiment, an example was shown in which the packing column 30 was used, but the packing column 30 may be omitted when the concentration of the slurry liquid is high or when the amount of packing into the packed column does not need to be the entire length of the column. be able to. Therefore, the small jack 34 for vertically moving this column can also be omitted. The procedure for loading the packing material when this packing column is omitted is to first load the rod 38a of the main jack 38.
is retracted to below the flange 10a at the lower end of the packed column 10, and in this state, the piston-shaped cap 36 is supported by the rod 38a at the lowest position of the packed column 10 (the position of the piston-shaped cap 36 shown by the solid line in FIG. 1). . After that, clamp 1
6, remove the cap 14, and perform the same operation as when using the packing column 30.

In the case of the downward pressing type shown in FIG. 7, the slurry is directly injected into the packed column 10, then a piston-shaped cap 36 is loaded, and the rod 38a of the main jack 38 is used to press the slurry.

In the present invention, as described above, packed column 10
A piston-like cap 36 is inserted into one end of the
This piston-shaped cap 36 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.

[Effects of the Invention] As is clear from the above explanation, according to the apparatus of the present invention, a packed column can be obtained without releasing the pressure after the high-pressure filling operation is completed, so a packed column can be obtained in which the high-pressure packing effect is maintained. It will be done. Further, it is possible to take out only packed columns, and it is also possible to obtain a large number of packed columns with one device. 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]

1 and 7 are longitudinal sectional views showing an embodiment of the device of the present invention, FIGS. 2, 3, and 5 are longitudinal sectional views of a piston-shaped cap, and FIG. A partial perspective view, FIG. 6 is a sectional view taken along the - line in FIG. 5. 10...Packed column, 12...Perforated plate, 14...
Cap, 24...Small jack, 30...Filling column, 36...Piston-shaped cap, 38...Main jack.

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 a packing material is loaded into the column, comprising: A packing column having approximately the same internal diameter as the chromatography column is detachably attached to one end of the chromatography column, and the cap on the one end side of the chromatography column passes through the packing column to fill the column. It is a piston-shaped member that can move into one end of the chromatography column, and can be locked to the inner wall surface of the chromatography column by protruding a projectable member provided on the side circumferential surface thereof. A chromatography apparatus comprising: a cap moving device that presses and moves the cap on the one end side through the packed column and into one end of the chromatography column.