JPH03113366A - Method and device for column-charging of high performance liquid chromatograph - Google Patents

Abstract

PURPOSE:To completely purge pressurized liquid which is small in specific gravity in a short time and to obtain a column with good column performance by putting a filler and slurry liquid in a packer and charging the filler in the column while feeding the pressurized liquid. CONSTITUTION:The column 2 is coupled with the packer 1, whose barrel part is held by a holder 3 and driven by a motor 5 through a rotating mechanism 4 to rotate. A selector valve 8 is placed on the side of the pressurized liquid A firstly and a liquid feed pump 7 is driven to charge the slurry liquid in the column 2 while admitting the liquid A from an intake 1a. Then the slurry liquid is discharged when fed by twice as much as the packer capacity and the pump 7 is stopped at the point of time when the liquid A remains; and the motor 5 is driven to rotate the whole packer 1 by 180 deg. and the valve 8 is switched to the side of liquid B, which is pressurized and fed. Then when the liquid B is fed by almost twice as much as the packer capacity, the pump 7 is stopped and the motor 5 is put in operation to switch the valve 8 to the side of the liquid A, which is charged in the column 2 again. Those operations are automated under the control of a control part 6.

Description

DETAILED DESCRIPTION OF THE INVENTION [Field of Industrial Application] The present invention relates to a column packing method and apparatus for a high performance liquid chromatograph used as a sample analysis device.

[Conventional technology]

In high performance liquid chromatography (hereinafter referred to as HPLC), the columns (most of which are made of stainless steel) that make up the apparatus are filled with a filler such as silica gel as a stationary phase. Dry photolithography was sometimes used as a column packing method, in which the filler is dropped little by little from the top using a funnel, etc., but this method is no longer used because particles smaller than 30 μm cannot be packed properly. Mostly, the wet method is used, in which the agent is dispersed in a solvent and filled under pressure. As shown in FIG. 4, such a filling device generally consists of a filling solvent H, a pump J, a pressure gauge with one flow adjustment knob, a packer M, a packed column N, and the like.

Conventionally, there are various methods for wet photothermography, but the typical method is to disperse silica gel in a solvent (e.g., tetrachloroethylene, liquid paraffin, etc.) to make a slurry liquid, transfer it to a packer, and pressurize it with a pressurizing liquid. There is a way to fill the column.

As for column packing conditions, ■slurry solvent composition (solvent for dispersing the filler), ■pressurized liquid, ■filling pressure or flow rate, ■purge liquid, ■direction in which the pressurized liquid flows, etc. have not been studied to the extent that There have been reports, but for columns that use an aqueous mobile phase (which currently accounts for about 80% or more), nothing has been established except for the use of methanol as the pressurizing liquid and the use of water as the purge liquid (both due to low cost). At present, there is no way to do this. Therefore, automated filling equipment is also not commercially available.

[Problem to be solved by the invention]

As described above, when purging the pressurized liquid in the column, in the conventional method, the pressurized liquid could not be completely removed and it took a long time. This is because the specific gravity of methanol, which is a pressurized liquid, is smaller than that of water, which is a purge liquid, and the pressurized liquid gathers at the top of the column, and if the inlet of the packer is placed upward, the pressurized liquid will not be pushed out, but will penetrate. This is because the pressurized liquid remains in the packer forever and the replacement (purging) of the remaining liquid is not successful.

Column performance has a large impact on analytical results, but HPL
For those who use C to analyze samples, how well the column is filled is extremely important. However, since column packing is often carried out by the analyst himself/herself, column performance and lifespan can vary considerably depending on the filling method and equipment, individual differences, and the performance of the filling equipment. This invention has been made to solve this problem.

[Means to solve the problem]

That is, in order to solve the above-mentioned problems, the present invention (1) stores a packing agent and a slurry liquid in a bunker that has a liquid inlet on one side for allowing a pressurized liquid and a purge liquid to flow in, and is connected to a column on the other side; In a high-performance liquid chromatograph column filling method in which the column is filled with a packing material while supplying a pressurized liquid, the bunker is held with a holder or arm, and the liquid inlet of the packer is initially directed upward. The column is filled with the filler and slurry liquid using a pump, and after a predetermined period of time, the filling is stopped and the rotation mechanism is used to rotate the bunker holder or arm to position the liquid inlet of the bunker downward. It is characterized by purging the pressurized liquid inside the packer.

(2) As a device for realizing the above means, a packer having a liquid inlet on one side for allowing a pressurized liquid or a purge liquid to flow in and connecting a column to the other side, and a holder or arm for holding the packer; A rotation mechanism that rotates the holder or arm, a switching valve that switches the flow of pressurized liquid and purge liquid into the packer, a pump that sends pressurized liquid and purge liquid into the packer, and these rotation mechanisms. It is characterized by a control section that controls the switching valve and the drive section of the pump.

[For production]

In method (2) above, after the slurry liquid is filled into the column, the slurry liquid is drained, but instead the pressurized liquid remains. However, the holder or arm is rotated using a rotating mechanism, the whole packer is turned upside down, and the liquid supply pump etc. The pressurized liquid can be purged almost completely by driving the purge liquid into the bunker from the bottom to the top. In other words, since the specific gravity of the pressurized liquid is smaller than the water in the purge liquid, when the inlet of the packer is placed upward, the pressurized liquid will not be pushed out but will penetrate through the packer, so the pressurized liquid will remain in the backer forever. Although the replacement (purging) of ``2'' does not work, this method can be used to successfully purge.

Furthermore, the apparatus means of item (1) above is optimal for implementing the method (2) and can automate the filling of the column.

〔Example〕

Hereinafter, specific embodiments of the present invention will be described with reference to the drawings.

FIG. 1 is a schematic diagram of an apparatus for carrying out the column filling method according to the present invention. In this figure, 1 is a packer, and a column 2 is connected to the lower part thereof, and this connection is made firmly so as to withstand high pressure. The body of the packer 1 is held by a holder 3, and the extranuclear holder 3 is rotated by a motor 5 (for example, a stamping motor) via a rotation mechanism 4. As the rotation mechanism 4, a mechanism that converts linear motion into rotational motion such as a rack and pinion, a rack and pin gear, or a lever crank mechanism, a rotary motion mechanism such as a gear and gears, a belt and a pulley, a cam mechanism, etc. are applied to the packer. 1 is a rotating mechanism that rotates 180 degrees. Further, the motor 5 is connected to and controlled by a controller (control unit) 6. 7 is a liquid sending pump,
A device with a maximum pressure of about 500 to 800 (kgf/cmz) is used, and a device capable of both constant pressure and constant flow liquid feeding is used. The liquid pump 7 is connected to and controlled by the control section 6. 8 is a switching valve for pressurized liquid A.
The purge liquid B (for example, water) can be switched to either the container 9 containing the liquid (for example, methanol) or the container 10 containing the purge liquid B (for example, water). Reference numeral 11 denotes a drive section for operating the switching valve 8, and the drive section 11 is also connected to and controlled by the control section 6. The pressurized liquid A and the purge liquid B are supplied to the switching valve 8, the liquid supply pump 7, and the microfilter 12.
The water flows into the packer 1 through the above. Note that the pipe 13 connecting these is made of stainless steel vibrator.

The structure of the apparatus used in the present invention is as described above, and next, the method of filling the column will be explained.

(1) First, as shown in FIG. 1, the packer 1 is placed so that the inlet port 1a faces upward, and the switching valve 8 is placed on the pressurized liquid A side. In this state, the liquid feed pump 7 is driven to introduce the pressurized liquid A from the inlet port 1a of the packer 1, and fill the column 2 with the slurry liquid.

Packer 1 is filled with a slurry liquid in which the filler is dispersed, but in order to shorten the filling time, a low viscosity solvent (for example, chloroform/methanol = 50150
) is used. In this case, since the specific gravity of chloroform is 1.48, which is larger than that of methanol, it is initially filled from top to bottom, and the liquid feed pump 7 is activated to push the slurry liquid with pressurized liquid A.

■Next, when twice the capacity of the packer is fed, the slurry liquid is drained and the pressurized liquid A remains in its place. Then, the entire packer 1 together with the holder 3 is rotated 180 degrees.

(2) In this state, the switching pulp operating section 11 is driven to switch the switching valve 8 to the purge liquid B side, and the liquid feeding pump 7 is driven to feed the purge liquid B into the packer I under pressure from the bottom to the top. In this way, the specific gravity of methanol, which is pressurized liquid A, is 0.79, and the specific gravity of water is 1, so methanol, which is pressurized liquid, remains in the upper part, but the inlet 1a of the bunker is positioned on the lower side. By flowing the purge liquid from the inside, the pressurized liquid can be easily discharged.

■After sending purge liquid B, which is about 3 times the packer capacity, stop the liquid pump 7, operate the motor 5, switch the switching valve 8 to the pressurized liquid A side, turn the packer 1 180 degrees or rotate it, and re-column the column. Perform step 2 filling.

The operation of filling columns 0 or more (1) to (2) is automated and controlled by the control unit 6.

FIG. 3 is a diagram showing the relationship between the change in filling pressure in the bunker 1 over time and the timing of packer rotation. One embodiment of the column filling method and apparatus according to the present invention is as described above, but in this embodiment, the motor 5 as a drive source for reversing or rotating the bunker 1 is replaced by another drive device,
For example, an air cylinder or a hydraulic cylinder that can be controlled by pneumatic pressure or hydraulic pressure may be used, or the packer 1 may be gripped by an arm and the arm itself may be configured to be able to reverse or rotate.

〔Effect of the invention〕

Since the column packing method and device according to the present invention are configured as described above, when a column is packed using this method and device, a pressurized liquid with a light specific gravity can be completely purged in a short period of time, and the detected peak can be completely purged in a short period of time. A column with good symmetry and good equicolumn performance can be obtained. Furthermore, it prevents deterioration of the column itself and extends its service life. Furthermore, with conventional methods, there were large variations in column performance, column life, etc., but reproducibility is also improved by automatic phototemperature.

4. Explanation of the drawings Fig. 1 is a schematic diagram of an apparatus for carrying out the column filling method according to the present invention, Fig. 2 is a diagram showing a state in which the packer is rotated 180 degrees to purge the pressurized liquid. FIG. 3 is a diagram showing the relationship between the temporal change in the filling pressure inside the packer and the timing of the packer rotation.

1- Bunker 2- Column 4- Rotating mechanism 5- Motor 6- Controller 7- Liquid pump 8- Switching pulp 9- Pressurized liquid container 10...
-・Purge liquid container 11・-・Switching valve drive unit

Claims (2)

[Claims] (1) Packing agent and slurry liquid are put into a packer that has a liquid inlet on one side for inflowing pressurized liquid and purge liquid, and is connected to a column on the other side, and while feeding pressurized liquid, it flows into the column. In a high-performance liquid chromatograph column filling method in which a packing agent is filled, the packer is held by a holder or an arm, and the liquid inlet of the packer is initially positioned upward, and a pump is used to pump the packing agent and slurry liquid. The column is filled, the filling is stopped after a predetermined period of time, and the packer holder or arm is rotated by a rotating mechanism to position the liquid inlet of the packer downward, thereby purging the pressurized liquid in the packer. Column packing method for high performance liquid chromatography. (2) A packer having a liquid inlet for pressurized liquid or purge liquid on one side and connected to a column on the other side, a holder or arm that holds the packer, and a rotation of the holder or arm. a switching mechanism for switching the flow of the pressurized liquid and the purge liquid into the packer, a pump for feeding the pressurized liquid and the purge liquid into the packer, and driving these rotation mechanisms, the switching valve, and the pump. A column packing device for a high performance liquid chromatograph, comprising: a control section for controlling a control section;