JPH0724726B2 - Liquid chromatograph column packing device - Google Patents

Description

Description: TECHNICAL FIELD The present invention relates to a packing device for a liquid chromatographic column, which packs a packing material into a liquid chromatographic column with high efficiency under pressure.

[Conventional technology]

In the conventional liquid chromatograph, the number of kinds of packing materials to be packed in the separation column, which is the main component, is small, and the packing method is also limited. However, recently, a large amount of biochemical substances and pharmaceuticals has been directed based on a separation-purification technique by liquid chromatography.
In order to carry out mass fractionation more efficiently, we use the most suitable packing material for the separation of the target substance, and use the column for liquid chromatograph that adopts the processing packing method that can further improve the separation efficiency of the column. It has come to be done. Usually, as a driving device for filling under pressure, there are a device utilizing a liquid pressure such as oil and gas, and a device using a mechanical transmission mechanism disclosed in Japanese Patent Laid-Open No. 61-7466.

[Problems to be solved by the invention]

However, the column packing devices that have been used so far have the following problems.

(1) In a device that pressurizes by using fluid pressure such as hydraulic pressure or gas pressure to increase the packing density of the filler, the movable plug is moved from the bottom to the top to be filled in relation to the working pressure. This is a method in which the entire filling material is filled under pressure into a fixed lid. In this case, since the whole particles of the packing material to be packed move, friction between the particles and the column wall or particles occurs,
As a result, the adsorption performance is deteriorated and the number of theoretical plates is reduced.

(2) An apparatus using a mechanical transmission mechanism injects a slurry-like filler into a column and then attaches a movable stopper to the column,
The movable plug is mechanically driven by using an electric motor or the like to pressurize the filler. However, when pressurizing the packing material, there was no mechanism to detect the optimum packing load according to the type of packing material and hold the packing load continuously, so it is necessary to improve the theoretical plate number of the column. It was

[Means for solving problems]

In view of the above problems, the present invention provides a column packing device for a liquid chromatograph that detects a packing load in order to apply an optimum packing load depending on the type of the packing, and continuously holds the packing load. To aim.

According to the present invention, a piston-shaped movable stopper having a movable stopper shaft is inserted from the upper end of the column into a column that is vertically fixed to a support base and has a cylindrical upper end, and a motor or the like is inserted. In a column packing device that press-fits a movable stopper downward from above the column by a mechanical transmission mechanism that is a drive source, the movable stopper shaft of the movable stopper and the mechanical transmission mechanism that presses the movable stopper shaft by the mechanical transmission mechanism are used. The connected drive shaft is vertically connected on the same axis and is connected in series, and the load applied to the packing material packed in the column between the upper end surface of the movable stopper shaft and the lower end surface of the drive shaft is Provided is a packing device for a column for a liquid chromatograph, which is provided with a load detector for detecting and a pressure holder for continuously holding the packing load.

[Action]

After injecting the slurry-like packing material whose concentration has been adjusted in advance into the column, the electric motor is operated to lower the movable stopper downward to pressurize the packing material. The indicated value of the load during pressurization is read to grasp the pressurization state, and when the load value reaches the optimum value for pressurizing and filling, the electric motor is stopped and the pressurizing and filling of the filler is completed. Further, in this pressurized state, the filling load is held by a pressure holding tool composed of a disc spring or the like.

〔Example〕

Next, a column packing device for a liquid chromatograph of the present invention will be described with reference to the drawings. In the column packing device for a liquid chromatograph shown in FIG. 1, an electric motor 1 having a sufficient capacity to pressurize the packing material is fixed to a support base 7, and a speed reducer 2 directly connected to the electric motor 1 is also a support base. It is attached to 7. A screw rod 12 is attached vertically above the speed reducer 2, and the screw rod 12 is rotated at a reduced speed via the speed reducer 2.

Adjacent to the screw rod 12, a support column 11 is fixed to the support base 7 and stands upright substantially in parallel. A screw rod 12 is screwed into a drive shaft mounting base 13 to which the drive shaft 14 is fixed. The drive shaft mounting base 13 is slidable in the upward and downward directions and does not rotate together with the screw rod 12. Is attached to the support pillar 11. The mechanical transmission mechanism refers to a series of power transmission mechanisms from the electric motor 1 to the drive shaft mount 13. The cylindrical column 9 is attached to the support base 7, the inside of the column 9 is filled with the packing material 10, and the movable plug 8 on which the movable plug shaft 15 is erected is arranged on the upper surface of the packing material 10. ing.

The capillary 6a passes through the shaft of the movable stopper shaft 15 and communicates with a filter (not shown) made of sintered metal or the like provided at the tip of the movable stopper 8, while under the other end of the column 9. The lid is also provided with a filter, and the capillary 6b communicates with this filter.

The drive shaft 14 is connected in series on the same axis as the movable stopper shaft 15 via the connecting tool 5.

The connecting device 5 includes a load detector 3 for detecting a filling load.
In addition, the pressure holding tool 4 that constantly holds the load and has elasticity is provided. There is a method of detecting the load by hydraulic pressure or the like for the load detector 3, but it is preferable to use a load cell to which a strain gauge is applied which can continuously detect the load and can indicate or record by an electric signal. The pressure holder 4 may be a spring having at least elasticity, but a disc spring that is small in bending and can withstand a large load is preferable. In Fig. 1, two disc springs are stacked in parallel, and four disc springs are combined in series. However, depending on the packing pressure required for the column packing device, the size of the device, etc. , The number of sheets, and the combination method may be selected.

Next, in order to fill the packing material into the column using the packing device of the present invention, the movable stopper 8 is raised above the support base 7 and the column 9 is fixed to the support base 7.

Then, after the slurry-like filler whose concentration has been adjusted in advance is injected into the column 9, the electric motor 1 is operated to lower the movable plug 8 to pressurize the filler 10. The liquid in the slurry-like filler is discharged to the outside through the capillaries 6a and 6b. During this pressure filling, the load instruction value of the load detector 3 is read, the load amount and the load speed are grasped, and the filling is performed under the optimum filling condition according to the type of the filler. When the final filling load is reached, the electric motor 1 is stopped. When the electric motor 1 is stopped,
Since the movable stopper remains in the stopped position, the filler 10 is pressed through the movable stopper 8 by the elastic force of the pressure holder 4. Capillary eluate under pressure
Flow to 6a or 6b to perform separation operation. It is also possible to provide a mechanism for automatically stopping the electric motor 1 when the final filling load is reached, so that the electric motor 1 is automatically stopped.

On the other hand, while the filling liquid is being injected from the capillaries 6a or 6b, the electric motor 1 may be operated and the movable plug 8 may pressurize the filling material.

〔The invention's effect〕

According to the present invention, by providing a load detector in a column packing device using a mechanical transmission mechanism, it is possible to know the optimum load velocity and final load during filling and pressurization according to the type of packing material, and also the elasticity. Since the pressure holding device having the above is used, the packing material can be continuously held in a pressurized state, and high-performance and high-speed separation can be performed using the column packed by this column packing device.

[Brief description of drawings]

FIG. 1 is a schematic configuration diagram showing a configuration example of a packing device for a liquid chromatograph column. In the figure, 1 is an electric motor, 2 is a speed reducer, 3 is a load detector, 4 is a pressure holder, 5 is a connecting tool, 6a and 6b are capillaries, 7 is a support, 8 is a movable stopper, 9 is a column, 10 is a filler, 11 is a support pillar, 12 is a screw rod, 13 is a drive shaft mount, and 14
Is a drive shaft, and 15 is a movable plug shaft.

Claims (3)

[Claims] 1. A column packing device for press-fitting a piston-shaped movable plug inserted into one end of a cylindrical column vertically fixed to a support base into the inside of the column by a mechanical transmission mechanism. The movable plug shaft and the drive shaft of the mechanical transmission mechanism are connected in series on the same axis, and a load detector for detecting the filling load between the upper end of the operating plug shaft and the lower end of the drive shaft and the filling load A packing device for a column for a liquid chromatograph, which is provided with a pressure holder for holding. 2. The packing device for a column for liquid chromatograph according to claim 1, wherein the load detector is a load cell. 3. The packing device for a column for liquid chromatograph according to claim 1 or 2, wherein the pressure holder is a disc spring.