JPH025412Y2 - - Google Patents

Description

[Detailed description of the invention] This invention relates to a large-scale liquid chromatography device for fractionating, purifying, concentrating, or separating a large amount of samples.In particular, the piston compression device has high filler filling efficiency and excellent reproducibility. The present invention relates to a liquid chromatography device of the type.

Conventionally, when a large amount of samples are purified, concentrated, or separated using a liquid chromatography device, a large-capacity column is used to increase the throughput per time, and the diameter is usually 10 to 200 mm and the length is 500 mm. ~
Columns of around 2000 mm are often used.

Even in such a liquid chromatography device for mass preparative use, it is desired that the column packing efficiency be as high as in a relatively small analytical chromatography device.

It is known that the filling efficiency is greatly influenced by the shape and particle size distribution of the filler as well as the filling method.

For analytical chromatography devices using columns with a diameter of about 2 to 8 mm, the conventional packing method is called the balanced slurry method, and uses a highly rigid packing material such as silica gel and a material with approximately the same specific gravity as the packing material. Using tetrabromoethane or methylene iodide as a dispersion medium and using a plunger pump etc.
There was a method of filling with a pressure of Kg/cm ² .

However, when this method is applied to a large-capacity column, the column and slurry storage tank must be highly pressure resistant, which results in an increase in the size of the entire device and the drawbacks of complicated operation and maintenance. It was hot.

Furthermore, since the dispersion medium is toxic, there is a safety problem.

On the other hand, the dry packing method applied to large-capacity columns does not use a solvent and only uses vibrating means such as a vibrator to fill the packing material, but this method does not offer much hope for improving the packing efficiency. Moreover, the reproducibility of the filling degree was poor.

Therefore, in Japanese Patent Application Laid-open No. 50-41595, the diameter is 50 mm.
A method has been proposed in which a piston is installed in a column with a large diameter of mm or more and the filler is compressed by the piston.

In this method, in order to fill the column with a highly rigid filler such as silica gel, the filler is mixed with an appropriate liquid to form a slurry, the slurry is injected into the column, and a porous filter is provided. The slurry was pressurized by a piston formed by the method, and the liquid component of the slurry was discharged to the outside of the column through the filter, thereby increasing the packing efficiency of the filler.

However, in this method, the piston is driven by hydraulic pressure or gas pressure, and requires a high-pressure gas cylinder or compressor, and furthermore, if the pressure is depressurized and then re-pressurized when the device is stopped,
There was a drawback that the filling degree of the filler varied and reproducibility decreased.

Furthermore, the overall size of the device has increased, and operation and maintenance have also tended to become more complicated.

The object of the present invention is to eliminate the drawbacks of the conventional methods and devices described above, and to provide a liquid chromatograph device with a compact structure, greatly improved packing efficiency, and high filling degree reproducibility.

The object of the present invention is to provide a cylindrical column; installed in the column, whose pressurizing surface is covered with a filter material, and is provided with a liquid collection groove and a drain port, while a thrust bearing is installed on the opposite side of the pressurizing surface. Attached piston member: Screw rod rotatably supported by the thrust bearing of the piston member: Its inner surface is covered with a filter material,
A bottom flange member of the column is provided with a liquid collection groove and a liquid drain port, and a desired compressive force is applied to the filler slurry injected into the column via the piston member, and the slurry is compressed. This is achieved by a liquid chromatograph apparatus characterized in that a liquid component is discharged to the outside of the column to maintain a constant filling degree of the packing material at all times.

Hereinafter, one embodiment of the device of the present invention will be described based on the attached drawings.

FIG. 1 is a longitudinal cross-sectional view of a main part 1 of the device according to the present invention, which includes a piston member 3 mounted inside a cylindrical column 2 so as to be able to reciprocate.

Further, the details of the structure of the column 2 and its surroundings are as follows.

Both end surfaces of the column 2 are provided with screw members 4 and 5, respectively.
It can be sealed by flanges 6 and 7 which are detachable.

A screw rod 8 is hinged to the center of the one flange 6 and passes through it, and the end of the screw rod 8 located inside the column 2 is rotatably pivoted by a thrust bearing 9 attached to the piston member 3. Since the other screw rod 8 is supported, the other screw rod 8 projects outwardly from the column 2.
When the end of the screw rod 8 is rotated with a spanner or wrench, the screw rod 8 is moved into the column 2.
It rotates and moves up and down along the axis C.

Therefore, the vertical movement of the screw rod 8 is transmitted to the piston member 3 through the thrust bearing 9, and the piston member 3 reciprocates within the column 2 together with the screw rod 8.

A ring-shaped seal 10 is fitted on the outer peripheral surface of the piston member 3, and the seal 10 seals a small gap between the inner peripheral surface of the column 2 and the outer peripheral surface of the piston member 3.

Further, the piston member 3 has a pressurizing surface 11 thereof.
As shown in FIG. 2, on the filling side of the column 2, a plurality of liquid collection grooves 13 are carved, which concentrate toward the liquid drainage port 12 that opens at a position offset from the center. The groove 13 is covered with a filter material 14 made of sintered metal or the like.

The drain port 12 serves as a drain flow path 15 and communicates with a drain pipe 16 that passes through the piston member 3 and extends outside the column 2.

Further, a drain port 17 is provided through the center of the inner surface of the other flange 7, and although not shown, the drain port 17 communicates with a suitable external drain pipe.

A plurality of liquid collection grooves 18 are carved on the inner surface of the flange 7 so as to concentrate polishing toward the liquid drainage port 17, and the liquid collection grooves 18 are formed by a filter material 19 made of sintered metal or the like. covered.

20 and 21 are packing members for each flange 6, 7.

The device 1 of the present invention configured as described above
After injecting a desired amount of slurry S obtained by mixing a relatively highly rigid filler such as silica gel with an appropriate liquid in advance into the column 2 from which the flange 6 and piston member 3 have been removed, The flange 6 and the piston member 3 are respectively attached to the predetermined positions.

Note that if you want to fill more easily, you may not remove the piston member 3, but invert the whole and remove the upwardly displaced flange 7, inject the slurry S, and then reinstall the flange 7. can.

After that, tighten the screw rod 8 with a spanner.
The slurry S is compressed through the piston member 3 by rotating using a jig such as a wrench. When the aforementioned slurry S starts to be compressed, the liquid contained in the slurry S flows through the filter material 14, the liquid collecting groove 13, the drain port 12, the drain channel 15, and the drain pipe 1.
They are pushed out of the container in the order of 6.

On the other hand, the liquid contained in the slurry S near the other flange 7 sequentially passes through the filter material 19, the liquid collection port 18, and the liquid drain port 17, and is discharged to the outside of the vessel.

Note that one of the drain pipes 16 and 17 is closed,
Excess liquid can also be drained from the other.

When the screwing torque of the screw rod 8 using the wrench or spanner reaches a predetermined value, in other words, when the compression force of the slurry S by the piston member 3 reaches a predetermined value, the tightening operation is stopped and the desired sample is purified. , perform concentration or separation treatment.

Even if the above-mentioned sample processing is interrupted, the apparatus of the present invention does not cause any change in the degree of filling of the slurry S, and can be reused even when left alone.

Of course, since there is no need to repeatedly activate and stop the pressurizing source, readjusting the filling degree of the slurry S can also be omitted.

Note that it is desirable that the inner surface of the column 2 in the device 1 of the present invention be lined with glass, stainless steel, or a synthetic resin such as Teflon.

Moreover, the piston member 3 and each flange 6, 7
Stainless steel, Hastelloy alloy, titanium, etc. are used.

Further, in order to uniformly discharge the liquid in the slurry S in the radial direction of the column 2 and to make the filling degree of the slurry S more uniform, each of the liquid drain ports 12,
17. It is possible to change the arrangement position and number of the liquid collection grooves 13 and 18 as appropriate.

Furthermore, instead of directly screwing the screw rod 8 onto the flange 6, a removable boss member is seated on the flange 6, and the screw rod 8 is screwed onto the boss member, so that the piston member 3 in the column 2 is not screwed directly onto the flange 6. It is also possible to perform the movement more quickly without removing the flange 6 or repeating the screwing operation.

Further, the liquid collection grooves 13 and 18 are not carved on the surfaces of the piston member 3 and the flange 7, but are formed between the piston member 3, the flange 7, and the filter material 1.
It is also possible to insert a suitable liner material between 4 and 19 and provide punched holes corresponding to the liquid collection grooves 13 and 18 described above in the liner material.

As described above, in the device of the present invention, the degree of filling of the slurry S can be controlled only by screwing in the screw rod 8.
Even when processing operations are stopped and restarted, there is no need to readjust the filling level due to stopping and restarting the pressurizing source, making it possible to easily maintain a constant filler filling level at all times. Ta.

Furthermore, it has become possible to provide an extremely compact device without requiring incidental equipment such as a high-pressure gas cylinder or compressor.

[Brief explanation of the drawing]

FIG. 1 is a longitudinal sectional view of the device of the present invention, and FIG. 2 is a bottom view of the piston member in the device of the present invention. 2 is a column, 3 is a piston member, 8 is a screw rod, 6 and 7 are flanges, and 14 and 19 are filter materials.

Claims (1)

[Claims for Utility Model Registration] Cylindrical column: installed in the column, its pressurized surface is covered with a filter material, and a liquid collection groove and drain port are provided, while a thrust bearing is installed on the opposite side of the pressurized surface. A piston member to which a screw rod is rotatably supported by a thrust bearing of the piston member: The inner surface of the screw rod is coated with a filter material,
A bottom flange member of the column is provided with a liquid collection groove and a liquid drain port, and a desired compressive force is applied to the filler slurry injected into the column via the piston member, and the slurry is compressed. A liquid chromatography apparatus characterized in that a liquid component is discharged to the outside of the column to maintain a constant filling degree of the packing material.