Method for automatically filling HPLC columns and automatic HPLC column filling apparatus

Abstract

The objective is to provide an automated method for loading HPLC columns and an automated HPLC column loading apparatus that can automate each step required when loading a packing material into an HPLC column. [Solution] An automatic HPLC column packing apparatus for automatically filling a packing material is provided, comprising: a pressure supply device for controlling the output of pressure inside the apparatus; a switching valve for adjusting the pressure inside the apparatus; a vent valve for adjusting the pressure inside the HPLC column packing apparatus, which has been pressurized or depressurized, to atmospheric pressure; a tank for storing a slurry containing the packing material; a solvent tank for storing a solvent; a packer, which is a container for supplying slurry to the HPLC column to fill it with the packing material; and a waste liquid tank for recovering excess slurry and / or solvent.

Description

Technical Field

[0001] The present invention relates to a method for automatically filling a column for high performance liquid chromatography (HPLC) with a filler, and an HPLC column automatic filling device for automatically filling a filler. More specifically, the present invention relates to a method for automatically filling an HPLC column and an HPLC column automatic filling device, which separately provide a conveyor for the HPLC column to be filled and can be driven at a higher pressure than conventional devices, and can automate each process required when filling a filler into an HPLC column.

Background Art

[0002] Columns used in HPLC (HPLC columns) are usually filled with a filler inside. As a problem with HPLC columns, individual differences may occur in the analysis performance and lifespan of HPLC columns. This is due to the fact that the analysis performance and lifespan of HPLC columns are determined by the filling degree of the filler, and the operation of filling the filler into the HPLC column is often performed by the HPLC operator himself / herself. Therefore, conventionally, attempts have been made to automate the operation of filling the filler into the column in order to achieve an HPLC column with a higher filling degree of the filler and no individual differences.

[0003] Patent Document 1 proposes a method and device for filling a column of high performance liquid chromatography. Specifically, Patent Document 1 provides a filling method and a filling device for solving the problem that there are significant variations in column performance and lifespan depending on individual differences and the performance of the filling device, by first filling the filler and the slurry liquid into the column with a pump while positioning the liquid flow inlet of the packer upward, stopping the filling after a predetermined time has elapsed, and using a rotating mechanism to position the liquid flow inlet of the packer downward to purge the pressurized liquid in the packer.

Prior Art Documents

Patent Documents

[0004] [Patent Document 1] Japanese Patent Application Publication No. 3-113366 [Overview of the project] [Problems that the invention aims to solve]

[0005] However, in order to achieve the production of HPLC columns that maintain a high level of packing density and have no variation in that density, it is desirable to achieve complete automation of every step of the packing process into the HPLC column by machine operation (i.e., no human intervention is required in the HPLC column packing process).

[0006] In view of the above circumstances, the present invention aims to provide an automatic method for filling an HPLC column with a packing material and an automatic HPLC column packing apparatus that can automate each step required when filling an HPLC column with a packing material. [Means for solving the problem]

[0007] The invention according to claim 1 relates to an automatic HPLC column packing apparatus for automatically packing a packing material, the apparatus comprising: a pressure supply device for controlling the output of pressure within the automatic HPLC column packing apparatus; a switching valve for adjusting the pressure within the automatic HPLC column packing apparatus; a vent valve for adjusting the pressurized or depressurized pressure within the automatic HPLC column packing apparatus to atmospheric pressure; a tank for storing a slurry containing a packing material; one or more solvent tanks for storing a solvent; a packer which is a container for storing the slurry containing the packing material supplied from the tank and the solvent tank by the pressure supply device, and for delivering the slurry to the HPLC column to pack the packing material; and a waste liquid tank for recovering excess slurry and / or solvent that overflows from the HPLC column when packing the HPLC column with the packing material.

[0008] The invention according to claim 2 further comprises a conveyor having the function of attaching and / or detaching the HPLC column to the packer, and is characterized in that it relates to the HPLC column automatic packing apparatus according to claim 1.

[0009] The invention according to claim 3 relates to the HPLC column automatic filling device according to claim 1, characterized in that the pressure supplied by the pressure supply device to the HPLC column automatic filling device is 200 MPa or less.

[0010] The invention according to claim 4 relates to the HPLC column automatic packing apparatus according to claim 1, further comprising a scraping member for scraping off excess slurry that has spilled out of the HPLC column after the packing material has been packed into the HPLC column.

[0011] The invention according to claim 5 relates to the HPLC column automatic packing apparatus according to claim 4, characterized in that the leveling member is made of an elastic material or resin.

[0012] The invention according to claim 6 is an automatic HPLC column packing apparatus according to any one of claims 1 to 5, further comprising a mounting unit for attaching a column end to the open end of the HPLC column after packing with the packing material.

[0013] The invention according to claim 7 relates to an HPLC column automatic filling apparatus according to claim 6, characterized in that the column end has a screw-in structure, and the mounting unit has a holding part for holding the column end and a rotational power supply part for rotating the holding part.

[0014] The invention according to claim 8 is a method for automatically filling an HPLC column with a packing material, the method comprising: (a) cleaning piping and / or packers arranged in an HPLC column automatic filling device used in the method; (b) attaching the HPLC column to a packer that functions as a container for filling the HPLC column with a packing material; (c) supplying a slurry containing the packing material to the packer by controlling the pressure using a pressure supply device; (d) supplying the slurry from the packer containing the slurry to the HPLC column by controlling the pressure using the pressure supply device; and (e) removing the HPLC column containing the packing material from the packer.

[0015] The invention according to claim 9 relates to the method of claim 8, characterized in that in step (b) and / or step (e), the HPLC column is attached to and / or removed from the packer by using a conveyor.

[0016] The invention according to claim 10 relates to the method according to claim 8, characterized in that the pressure supplied by the pressure supply device to the HPLC column automatic filling device is 200 MPa or less.

[0017] The invention according to claim 11 relates to the method of 8, further comprising a step of scraping off excess slurry that is protruding from the HPLC column between step (d) and step (e).

[0018] The invention according to claim 12 relates to the method according to claim 11, characterized in that, in the step of scraping off the excess slurry, after the HPLC column is placed on the transporter, the transporter is moved so that it passes under a fixed scraping member, thereby scraping off the excess slurry.

[0019] The invention according to claim 13 relates to the method of claim 12, further comprising the step of attaching a column end to the open end of the HPLC column between the step of scraping off the excess slurry and step (e).

[0020] The invention according to claim 14 relates to the method according to claim 13, characterized in that, in the step of attaching the column end, the column end having a screw-in structure is attached to the open end of the HPLC column by rotating and pushing it in.

[0021] The invention according to claim 15 relates to an automatic HPLC column packing apparatus used in the method according to any one of claims 8 to 14, for automatically packing a packing material, the apparatus comprising: a pressure supply device for controlling the pressure inside the automatic HPLC column packing apparatus; a switching valve for adjusting the pressure inside the automatic HPLC column packing apparatus; a vent valve for adjusting the pressurized or depressurized pressure inside the automatic HPLC column packing apparatus to atmospheric pressure; a tank for storing a slurry containing a packing material; one or more solvent tanks for storing a solvent; a packer which is a container for storing the slurry containing the packing material supplied from the tank and the solvent tank by the pressure supply device, and for delivering the slurry to an HPLC column to pack the packing material; a waste liquid tank for recovering excess slurry and / or solvent that overflows from the HPLC column when packing the HPLC column with the packing material; and a conveyor having the function of attaching and / or detaching the HPLC column to the packer.

[0022] The invention according to claim 16 relates to the HPLC column automatic packing apparatus according to claim 15, further comprising a conveyor having the function of attaching and / or detaching the HPLC column to the packer. [Effects of the Invention]

[0023] According to the invention of claim 1, there is provided an automatic column filling device for HPLC for automatically filling packed materials, the device comprising: a pressure supply device for controlling the output of pressure within the automatic column filling device for HPLC; a switching valve for adjusting the pressure within the automatic column filling device for HPLC; a vent valve for adjusting the pressure within the automatic column filling device for HPLC, which has been pressurized or depressurized, to normal pressure; a tank for storing a slurry containing the packed material; one or more solvent tanks for storing a solvent; a packer which is a container for storing the slurry containing the packed material supplied by the pressure supply device from the tank and the solvent tank and for feeding the slurry to the HPLC column to fill the column with the packed material; and a waste liquid tank for recovering excess slurry and / or solvent overflowing from the HPLC column when filling the column with the packed material. Therefore, since it is an automatic column filling device for HPLC, it is possible to provide an automatic column filling device for HPLC that can automate each process required when filling a packed material into an HPLC column.

[0024] According to the invention of claim 2, the automatic column filling device for HPLC according to claim 1 further comprises a transporter having a function of attaching and / or detaching the HPLC column to / from the packer. Therefore, by separately providing a transporter for the HPLC column to be filled, it is possible to provide an automatic column filling device for HPLC that can automatically attach an unfilled HPLC column to the filling device and / or automatically detach the filled HPLC column from the filling device without an operator intervening in the HPLC column filling operation (here, manual attachment and detachment of the HPLC column by the operator).

[0025] According to the invention according to claim 3, the pressure provided by the pressure supply device to the HPLC column automatic filling device is 200 MPa or less. The HPLC column automatic filling device according to claim 1 is characterized in that by driving at a higher pressure than the conventional device, it is possible to provide an HPLC column automatic filling device capable of automating each process necessary for filling the packing material into the HPLC column.

[0026] According to the invention according to claim 4, after filling the packing material into the HPLC column, the HPLC column automatic filling device according to claim 1 further comprises a scraping member for scraping off the excess slurry protruding from the HPLC column. By scraping off the excess slurry with the scraping member, the amount of the packing material filled into the HPLC column can be made more uniform.

[0027] According to the invention according to claim 5, the scraping member is made of an elastic body or resin. The HPLC column automatic filling device according to claim 4 is characterized in that it is possible to suppress damage to the HPLC column when scraping off the excess slurry with the scraping member.

[0028] According to the invention according to claim 6, the HPLC column automatic filling device according to any one of claims 1 to 5 further comprises an attachment unit for attaching a column end to the open end of the HPLC column after filling the packing material. Thus, the attachment of the column end to the HPLC column can also be performed automatically.

[0029] According to the invention according to claim 7, the column end has a screw-in structure, and the attachment unit has a holding part for holding the column end and a rotational power supply part for rotating the holding part. The HPLC column automatic filling device according to claim 6 is characterized in that by rotating the holding part by the rotational power supply part, the column end held by the holding part can be screwed into the open end of the HPLC column.

[0030] According to the invention of claim 8, there is an automatic method for filling an HPLC column with a packing material, the method comprising: (a) cleaning piping and / or packers arranged in an automatic HPLC column filling device used in the method; (b) attaching the HPLC column to a packer that functions as a container for filling the HPLC column with a packing material; (c) supplying a slurry containing the packing material to the packer by controlling the pressure using a pressure supply device; (d) supplying the slurry from the packer containing the slurry to the HPLC column by controlling the pressure using the pressure supply device; and (e) removing the HPLC column containing the packing material from the packer. Therefore, an automatic HPLC column filling method is provided that automates each step necessary when filling an HPLC column with a packing material.

[0031] The invention according to claim 9 is characterized in that, in step (b) and / or step (e), the HPLC column is attached to and / or removed from the packer by using a conveyor. Therefore, by further using a conveyor for the HPLC column to be filled in this method, it is possible to provide an automated HPLC column filling method in which an unfilled HPLC column can be automatically attached to the filling device and / or a filled HPLC column can be automatically removed from the filling device without the operator having to intervene in the HPLC column filling operation (in this case, manual attachment and removal of the HPLC column by the operator).

[0032] According to the invention of claim 10, the method according to claim 8 is characterized in that the pressure supplied by the pressure supply device to the HPLC column automatic filling device is 200 MPa or less. Therefore, by driving with high pressure, it is possible to provide an HPLC column automatic filling method that can automate each step necessary when filling the HPLC column with packing material.

[0033] The invention according to claim 11 is characterized in that the method according to claim 8 further includes a step of scraping off excess slurry that is protruding from the HPLC column between step (d) and step (e), so that by scraping off the excess slurry, the amount of packing material packed into the HPLC column can be made more uniform.

[0034] According to the invention of claim 12, in the step of scraping off the excess slurry, after the HPLC column is placed on the transporter, the transporter is moved and passed under the fixed scraping member, thereby scraping off the excess slurry. This method of claim 11 allows for automatic scraping off of the excess slurry by moving the transporter, and also suppresses variations in the scraping process.

[0035] The invention according to claim 13 is characterized in that the method according to claim 12 further includes a step of attaching a column end to the open end of the HPLC column between the step of scraping off the excess slurry and step (e), so that the attachment of the column end to the HPLC column can also be performed automatically.

[0036] According to the invention of claim 14, the method of claim 13 is characterized in that, in the step of attaching the column end, the column end having a screw-in structure is attached to the open end of the HPLC column by rotating and pushing it in. Therefore, the column end can be reliably attached by screwing it onto the open end of the HPLC column.

[0037] According to the invention of claim 15, an HPLC column automatic filling apparatus used in the method of any one of claims 8 to 14, which automatically fills a packing material, the apparatus comprising: a pressure supply device for controlling the pressure inside the HPLC column automatic filling apparatus; a switching valve for adjusting the pressure inside the HPLC column automatic filling apparatus; a vent valve for adjusting the pressurized or depressurized pressure inside the HPLC column automatic filling apparatus to atmospheric pressure; a tank for storing a slurry containing a packing material; one or more solvent tanks for storing a solvent; a packer which is a container for storing the slurry containing the packing material supplied from the tank and the solvent tank by the pressure supply device, and for delivering the slurry to the HPLC column to fill the packing material; and a waste liquid tank for recovering excess slurry and / or solvent that overflows from the HPLC column when filling the HPLC column with the packing material, the apparatus provides a filling apparatus that can perform an HPLC column automatic filling method that automates each step necessary when filling an HPLC column with a packing material.

[0038] The invention according to claim 16 is characterized by further comprising a conveyor having the function of attaching and / or removing the HPLC column to the packer, and is therefore an automatic HPLC column filling device according to claim 15. By separately providing a conveyor for the HPLC column to be filled, it is possible to provide an automatic HPLC column filling device that can automatically attach an unfilled HPLC column to the filling device and / or automatically remove a filled HPLC column from the filling device without the operator having to intervene in the HPLC column filling operation (in this case, manual attachment and removal of the HPLC column by the operator). [Brief explanation of the drawing]

[0039] [Figure 1] This figure shows the step of cleaning the piping and / or packer in the method for automatically filling an HPLC column according to the present invention. [Figure 2] This figure shows the preparation stage for filling an HPLC column with packing material in the method for automatically packing an HPLC column according to the present invention. [Figure 3] This figure shows the step of filling an HPLC column with packing material in the method for automatically packing an HPLC column according to the present invention. [Figure 4] This figure shows the stage after the packing of the packing material into the HPLC column has been completed in the method for automatically packing an HPLC column according to the present invention. [Figure 5] This figure shows one embodiment of the conveying machine according to the present invention. [Figure 6] This diagram illustrates the process of trimming off excess packing material protruding from an HPLC column, where (a) shows an HPLC column filled with packing material placed in a transport stocker, (b) shows the HPLC column placed in the transport stocker being moved toward a trimming member, (c) shows the excess slurry protruding from the HPLC column in contact with the trimming member, and (d) shows the HPLC column after the excess slurry has been trimmed by the trimming member. [Figure 7] This diagram illustrates the process of attaching a column end to the open end of an HPLC column, where (a) shows the HPLC column, the column end, and the attachment unit; (b) shows the state in which the column end is held by the holding part of the attachment unit; (c) shows the state in which the column end has been moved to an upper position on the HPLC column by the holding part; and (d) shows the state in which the column end is attached to the open end of the HPLC column. [Modes for carrying out the invention]

[0040] The following describes in detail, with reference to the drawings, an embodiment of the method for automatically filling an HPLC column and an automatic HPLC column filling apparatus according to the present invention. However, the technical scope of the present invention, as well as the numerical values ​​and numerical ranges described herein, should not be limited by these descriptions.

[0041] Figures 1 to 4 illustrate a method for automatically packing an HPLC column. Specifically, Figure 1 shows the process of cleaning the piping and / or packer 7 in the method for automatically packing an HPLC column. Figure 2 shows the preparation stage for packing the HPLC column with packing material in the method for automatically packing an HPLC column. Figure 3 shows the stage of packing the HPLC column with packing material in the method for automatically packing an HPLC column. Figure 4 shows the stage after the packing of the HPLC column with packing material has been completed in the method for automatically packing an HPLC column.

[0042] The method for automatically filling an HPLC column 10 according to the present invention is characterized by comprising the steps of: (a) cleaning the piping and / or packer 7 arranged in the apparatus used for the filling method (Figure 1); (b) attaching the HPLC column 10 to the packer 7, which functions as a container for filling the HPLC column 10 with packing material, using a conveyor 11 (Figure 2); (c) supplying a slurry containing packing material to the packer 7 by controlling the pressure using a pressure supply device 2a (Figure 3); (d) supplying slurry from the packer 7 containing the slurry to the HPLC column 10 by controlling the pressure using a pressure supply device 2a (Figure 3); and (e) removing the HPLC column 10 containing the packing material from the packer 7 using a conveyor 11 (Figure 4). Although the use of the conveyor 11 is described in steps (b) and (e), it is not necessarily required to use the conveyor 11 in any of these steps. For example, the HPLC column 10 can be attached to and / or removed from the packer 7 manually by an operator.

[0043] In the process of cleaning the piping and / or packer 7 in the automated packing method for the HPLC column 10 shown in Figure 1, the water levels of tank 5 and solvent tank 6 are first checked, and then the pressure supply device 2b and agitator are activated. Next, the solvent in solvent tank 6, which contains the solvent selected as the cleaning solution for cleaning the piping and / or packer 7, is drawn out using the pressure supply device 2a to clean the piping and / or packer 7. When a sensor (e.g., a level sensor) detects the liquid level in waste tank 8, the pressure supply device 2a is stopped and the pressure supply device 2c is activated to collect the remaining liquid in packer 7 into waste tank 8.

[0044] In the process of attaching the HPLC column 10 to the packer 7, which functions as a container for filling the HPLC column 10 with packing material, as shown in Figure 2, the cylinder 9 is pushed out and the conveyor 11 moves the HPLC column 10 below the packer 7. After the movement, the cylinder 9 is retracted, which creates a pressure reduction, allowing the HPLC column 10 to be pressed and fixed to the packer 7. Here, moving the HPLC column 10 below the packer 7 and pressing and fixing the HPLC column 10 to the packer 7 by retracting the cylinder 9 can also be done manually, for example, by an operator, without using the conveyor 11. Subsequently, by operating the switching valve 3, slurry can be delivered to the packer 7. The amount delivered is the amount of slurry to be put into the packer 7, which was set by the operator during the preparation, and this amount of slurry is delivered to the packer 7 while managing the time. After the slurry is delivered to packer 7, the solvent contained in the slurry is delivered to packer 7 by pushing the switching valve 3 so that the solvent contained in the slurry fills the empty space in packer 7. Then, when a sensor (e.g., a level sensor) detects a rise in the liquid level of waste liquid tank 8, the gas release valve 4 is operated to create a closed space within the device circuit including packer 7, and it is confirmed that the inside of the device including packer 7 is pressurized. The agitator is stopped once and the slurry level in tank 5 is checked, for example, using a sensor. Then the agitator is restarted.

[0045] In the process shown in Figure 3, which involves supplying a slurry containing packing material to a packer 7 and then supplying the slurry from the packer 7 to the HPLC column 10 by controlling the pressure using a pressure supply device 2a, the slurry is supplied from the packer 7 to the HPLC column 10 while checking the rising pressure and the maintained pressure using sensors (e.g., pressure sensors) to determine whether the set rising pressure and the time it takes to rise that pressure have been achieved, and whether the set maintenance pressure and the time it takes to maintain that pressure have been achieved, thereby filling the HPLC column 10 with packing material. After that, the pressure supply device 2a is stopped and the system waits until the pressure inside the packer 7 is reduced to a reduced state, preferably, for example, 0.1 MPa or less. After confirming that the pressure has been reduced, the gas release valve 4 is operated to return the pressure inside the packer 7 to atmospheric pressure. After returning to atmospheric pressure, the pressure supply device 2c is activated to collect the remaining liquid inside the packer 7 and the HPLC column 10 attached to the packer 7 into the waste liquid tank 8.

[0046] In the process of removing the HPLC column 10 containing the packing material from the packer 7, as shown in Figure 4, the cylinder 9 is pushed out, and the HPLC column 10 filled with the packing material is recovered by the conveyor 11 and moved to the storage location for the filled HPLC column 10. This completes the automatic packing method for the HPLC column 10. Hereinafter, the process of pushing out the cylinder 9 to recover the HPLC column 10 filled with the packing material, and moving the filled HPLC column 10 to the storage location for the filled HPLC column 10, can also be done manually, for example, by an operator, without using the conveyor 11. After that, after preliminary preparations, the process of cleaning the piping and / or packer 7, as already shown in Figure 1, can be started again.

[0047] The method for automatically packing an HPLC column according to the present invention may further include a step of scraping off any excess slurry protruding from the HPLC column 10 between the step of supplying slurry from the packer 7 to the HPLC column 10 (d) and the step of removing the HPLC column 10 containing the packing material from the packer 7 (e).

[0048] Figure 6 illustrates the process of scraping off excess slurry that is protruding from the HPLC column 10. Figure 6(a) shows the HPLC column 10, which is packed with packing material, placed in the transport stocker 22, which is a transporter. As shown in Figure 6(a), in the state in which the packing material is packed into the HPLC column 10 in step (d), excess slurry 21 may protrude from the open end 10a of the HPLC column 10.

[0049] The transport stocker 22 is a transport unit for transporting HPLC columns 10 filled with packing material to a location for the next process, and is configured to accommodate multiple HPLC columns 10. In the example shown in Figure 6, the transport stocker 22 is provided with recesses for HPLC columns 10, and the HPLC columns 10 are installed by inserting them into the recesses. However, the HPLC columns 10 can be installed in the transport stocker 22 by any method as long as the HPLC columns 10 are fixed in place.

[0050] In the step of scraping off excess slurry 21, after placing the HPLC column 10 in the transport stocker 22, the transport stocker 22 is moved and passed under the fixed scraping member 23 to scrape off the excess slurry 21. Figure 6(b) shows the state in which the HPLC column 10 placed in the transport stocker 22 is being moved toward the scraping member 23. There are no particular restrictions on the method of moving the transport stocker 22, and it can be moved in any way. For example, the transport stocker 22 is configured to be rotatable horizontally by a motor. In this case, the transport stocker 22 moves in the rotational direction.

[0051] The leveling member 23 is a member for leveling off excess slurry 21 that protrudes from the HPLC column 10, and is fixed in a predetermined position. The leveling member 23 is made of an elastic material such as rubber or a resin. The resin preferably has chemical resistance that prevents degradation even when in contact with the slurry containing the packing material, and is, for example, PEEK or PTFE. By making the leveling member 23 out of an elastic material or a resin, damage to the HPLC column 10 can be suppressed when the leveling member 23 levels off the excess slurry 21. The leveling member 23 is, for example, a plate, but its shape is not limited to a plate and can be any shape.

[0052] Figure 6(c) shows the state in which the excess slurry 21 overflowing from the HPLC column 10 comes into contact with the leveling member 23 as the transport stocker 22 moves. As the transport stocker 22 moves, the HPLC column 10 passes under the leveling member 23, and the excess slurry 21 is leveled off by the leveling member 23. For this reason, the leveling member 23 is fixed in a position that allows it to level off the excess slurry 21 overflowing from the HPLC column 10.

[0053] Figure 6(d) shows an HPLC column 10 with excess slurry 21 leveled off after passing under the leveling member 23. By leveling off the excess slurry 21 with the leveling member 23, the amount of packing material packed into the HPLC column 10 can be made more uniform. Furthermore, by moving the transport stocker 22 on which the HPLC column 10 is installed, the excess slurry 21 can be leveled off automatically, and variations in leveling can be suppressed compared to when leveling is done manually by a person.

[0054] The method for automatically packing an HPLC column according to the present invention may further include a step of attaching a column end to the open end 10a of the HPLC column 10 between the step of scraping off excess slurry 21 and the step of removing the HPLC column 10 containing the packing material from the packer 7 (e). However, if the step of scraping off excess slurry 21 is not performed, the step of attaching a column end to the open end 10a of the HPLC column 10 is performed between step (d) and step (e).

[0055] Figure 7 illustrates the process of attaching a column end 31 to the open end 10a of an HPLC column 10. Figure 7(a) shows the HPLC column 10, the column end 31, and the attachment unit 32. The attachment unit 32 is for attaching the column end 31 to the open end 10a of the HPLC column 10 after packing with packing material, and has a holding part 33 for holding the column end 31 and a rotational power supply part 34 for rotating the holding part 33. The rotational power supply part 34 is, for example, a motor. However, the rotational power supply part 34 can be anything that can supply rotational power to rotate the holding part 33, for example, an air turbine.

[0056] The column end 31 has a screw-in structure. Specifically, the inner surface of the column end 31 is threaded (internal thread), and it is configured to be screwed into the HPLC column 10, which has threaded (external thread) on the outer surface of the open end 10a.

[0057] Figure 7(b) shows the state in which the column end 31 is held by the holding part 33 of the mounting unit 32. For example, the mounting unit 32 is configured so that the holding part 33 can be moved in the vertical and horizontal directions. In order to hold the column end 31, the mounting unit 32 moves the holding part 33 from a predetermined standby position to the position where the column end 31 is placed. The holding part 33 has an arm 33a, as shown in Figure 7(a), and the column end 31 is held by the arm 33a.

[0058] When the holding part 33 holds the column end 31, the mounting unit 32 moves the holding part 33 so that the column end 31 is positioned above the HPLC column 10. Figure 7(c) shows the state in which the holding part 33 has moved the column end 31 to a position above the HPLC column 10.

[0059] Next, the mounting unit 32 lowers the holding part 33 until the column end 31 covers the open end 10a of the HPLC column 10, and then lowers the holding part 33 further while driving the rotary power supply unit 34. By driving the rotary power supply unit 34, the holding part 33 rotates and lowers the holding part 33 further, so that the column end 31 held by the holding part 33 is screwed onto the open end 10a of the HPLC column 10. In other words, the column end 31, which has a screw-in structure, is attached to the open end 10a of the HPLC column 10 by rotating and pushing it in. Figure 7(d) shows the state in which the column end 31 is attached to the open end 10a of the HPLC column 10.

[0060] When the column end 31 is attached to the open end 10a of the HPLC column 10, the holding part 33 releases its grip on the column end 31 and moves the holding part 33 to a predetermined standby position.

[0061] As preliminary preparations for performing the automatic packing method for HPLC columns 10 according to the present invention, the following should be noted: (1) Check the remaining volume of tank 5 and solvent tank 6. This can be done, for example, by using a sensor to check the water level of the liquid (in this case, slurry containing packing material or solvent) in tank 5 or solvent tank 6, or by using a sensor (e.g., a weight sensor) to check the weight of the liquid in tank 5 or solvent tank 6, and replenishing the liquid (in this case, slurry containing packing material or solvent) as needed. (2) Set whether or not to use solvent tank 6. In this invention, one or more solvent tanks 6 can be used (although two solvent tanks 6 are shown in Figures 1 to 4, it is possible to use two or more), so if multiple solvent tanks 6 are connected to the HPLC column automatic packing device 1, the solvent tank 6 to be used can be selected from among them. (3) If using the conveyor 11, check, for example, using a proximity sensor, whether the HPLC column 10 for packing is connected to the conveyor 11. (4) Confirm that the input air pressure is, for example, 0.2 MPa or higher. (5) Check the set value and change it as needed. For example, these include the amount (ml) of liquid to be used (in this case, slurry containing packing material or solvent), the amount of slurry to be put into packer 7 (ml), the selection of a cleaning solution for cleaning the piping and / or packer 7 (the cleaning solution is selected from the solvents in solvent tank 6), the selection of a solvent to be included in the slurry (the solvent to be included in the slurry is selected from the solvents in solvent tank 6, similar to the cleaning solution), the rising pressure (MPa), the time (min) for the pressure to rise to reach that rising pressure, the maintenance pressure (MPa), and the maintenance time (min) of that maintenance pressure. However, if the automatic packing method for the HPLC column 10 according to the present invention can be performed without problems, it is not necessary to set all of these values. All or part of the operation of the method and apparatus according to the present invention, including this preparation, may be performed, for example, by operating a control panel connected to operate the HPLC column automatic packing apparatus 1 using the method.

[0062] An HPLC column automatic packing apparatus 1 using the method for automatically packing an HPLC column 10 according to the present invention comprises a pressure supply device (2a, 2b, 2c) for controlling the output pressure within the apparatus, a switching valve 3 for adjusting the pressure within the apparatus, a vent valve 4 for adjusting the pressurized or depressurized pressure within the HPLC column automatic packing apparatus 1 to, for example, atmospheric pressure, a tank 5 for storing a slurry containing packing material, one or more solvent tanks 6 for storing solvent, a packer 7 which is a container that stores the slurry containing packing material supplied from the tank 5 and solvent tanks 6 by the pressure supply device (2a, 2b, 2c) and functions to deliver the slurry to the HPLC column 10 to pack the packing material, and a waste liquid tank 8 for recovering excess slurry and / or solvent that overflows from the HPLC column 10 when packing the HPLC column 10 with packing material. The HPLC column automatic packing apparatus 1 according to the present invention can output high pressure when delivering slurry and solvent to the packer 7 and the like. The operator of the present invention may optionally use a conveyor 11 that has the function of attaching and / or detaching the HPLC column 10 to the packer 7.

[0063] Unlike conventional HPLC column automatic packing systems, the pressure supply devices (2a, 2b, 2c) according to the present invention can provide high pressure to the HPLC column automatic packing system 1. To achieve this high pressure, a switching valve 3 for adjusting the pressure inside the system 1 and a vent valve 4 for adjusting the pressure inside the system 1 to, for example, atmospheric pressure are required.

[0064] Preferably, the performance of the switching valve 3 includes, for example, a maximum supply air pressure of 0.7 (MPa), and a theoretical air cylinder output of 3520 (N) for extrusion and 3170 (N) for retraction. The switching valve 3 preferably includes a section for supplying slurry to the packer 7, a section used for pressurizing when supplying slurry to the HPLC column 10, the maximum supply pressure of which may be, for example, approximately 115, 200, or 300 (MPa), a section for use as a slurry outlet, and a section for connection to the packer 7.

[0065] For the performance of the gas vent valve 4, for example, a maximum supply air pressure of 0.7 (MPa) and a theoretical air cylinder output of 3520 (N) for extrusion and 3170 (N) for retraction are preferred. The gas vent valve 4 is preferably provided with a portion used for pressurizing when supplying slurry to the HPLC column 10, and which is suitable even if the maximum pressure inside the piping is, for example, about 115, about 200, or about 300 (MPa).

[0066] The HPLC column automatic filling apparatus 1 according to the present invention is equipped with equipment that is driven by air (e.g., a switching valve 3, a vent valve 4, and a cylinder 9) as its driving source. However, if each of the processes required to fill the HPLC column 10 with packing material can be automated, the driving source can be replaced with, for example, electricity or hydraulics.

[0067] The pressure supply devices 2a, 2b, or 2c are devices used to adjust the pressure inside the HPLC column automatic packing apparatus 1 to any desired pressure, and the type of device can be arbitrarily set by the operator of the present invention, as long as it can be used for either pressurizing or depressurizing.

[0068] Tank 5 has the function of storing slurry and is equipped with a stirrer to agitate the slurry inside Tank 5. Slurry is transferred from Tank 5 to Packer 7, and the slurry transferred to Packer 7 is then transferred to HPLC column 10 to fill it with packing material. Therefore, it is preferable to further provide a sensor so that the operator of the present invention can know the remaining amount of slurry in Tank 5.

[0069] The solvent tank 6 has the function of storing the solvent and washing solution contained in the slurry. Since the present invention is intended to use multiple types of liquids, it is preferable that the HPLC column automatic packing device 1 be equipped with two or more solvent tanks 6. However, since the washing solution and the solvent contained in the slurry can be of the same type, it is also possible to install only one solvent tank 6.

[0070] Packer 7 is used to deliver slurry from tank 5 to an empty HPLC column 10 and fill it with packing material. Packer 7 is linked to cylinder 9, and the empty HPLC column 10 can be compressed and fixed by pulling in cylinder 9. After the HPLC column 10 is filled with packing material, the filled HPLC column 10 can be removed from packer 7 by pushing out cylinder 9.

[0071] The waste liquid tank 8 is a tank that collects waste liquid generated after cleaning the piping and / or packer 7 in the HPLC column automatic packing device 1, as well as residual solvents, slurries, and other liquids generated when packing the HPLC column 10 with packing material.

[0072] A slurry is a mixture in which solid particles are suspended in a liquid. In this invention, a slurry is described as a mixture containing a packing agent and a solvent suitable for HPLC, which is delivered to an HPLC column 10 to pack the column with the packing agent.

[0073] As fillers, for example, silica gel, polymer gel, zirconia, and fillers in which the surface of silica gel has been surface-treated with octadecylsilyl groups can be used, but the specific filler used will be arbitrarily determined by the operator of this invention depending on the sample to be analyzed.

[0074] For example, water, alcohol (methanol, ethanol, etc.), and acetonitrile are used as solvents or washing solutions suitable for HPLC. However, depending on the sample to be analyzed, the appropriate solvent for HPLC analysis and the appropriate washing solution for cleaning the piping and / or packer 7 will be arbitrarily set by the operator of the present invention before analysis, due to different circumstances.

[0075] The pressure supply devices (2a, 2b, 2c) in the HPLC column automatic packing apparatus 1 according to the present invention can provide a pressure of about 1 MPa or more and about 300 MPa or less, preferably about 200 MPa or less, but can be arbitrarily changed by the operator. The HPLC column automatic packing apparatus 1 according to the present invention can output high pressure when supplying slurry or solvent to packer 7, etc. By outputting high pressure, for example, the operator can control the packing speed to packer 7 and HPLC column 10, and as a result can control the respective packing times.

[0076] Here, "approximately" indicates that the numbers listed after "approximately" include numbers within a 10% range. For example, "approximately 200" refers to numbers between 180 and 220, and "approximately 50" refers to numbers between 45 and 55.

[0077] Figure 5 shows one embodiment of the conveyor 11 according to the present invention. The conveyor 11 according to the present invention is described as a device equipped with a cylinder 12 and air-driven equipment (actuator 13, chuck 14), which has the function of moving the HPLC column 10 before packing material is placed under the packer 7 and attaching the HPLC column 10 before packing material is placed under the packer 7, and the function of automatically removing the HPLC column 10 after packing material is placed under the packer 7 and automatically moving it to the place where the HPLC column 10 after packing material is placed. The conveyor 11 according to the present invention only needs to have the function of moving the HPLC column 10 before packing material is placed under the packer 7 and attaching the HPLC column 10 to the packer 7, and the function of automatically removing the HPLC column 10 after packing material is placed under the packer 7 and automatically moving it to the place where the HPLC column 10 after packing material is placed, and is not limited to the embodiment shown in Figure 5. For example, the conveyor 11 can be replaced with one driven by electricity or hydraulics, or the HPLC column 10 can be moved to below the packer 7 by a belt conveyor, and then the HPLC column 10 can be attached or detached by robotic operation (automatic), such as by a robotic arm, and then automatically moved by the belt conveyor to the storage location of the filled HPLC column 10. [Industrial applicability]

[0078] The method for automatically filling an HPLC column 10 and the HPLC column automatic filling apparatus 1 according to the present invention can automate each step required when filling the HPLC column 10 with packing material, and is therefore useful for manufacturers related to chemical analysis, especially HPLC, as well as analytical institutions and research institutions that perform sample analysis or research. [Explanation of symbols]

[0079] 1. Automatic column packing system for HPLC 2a, 2b, 2c Pressure supply device 3. Diverter valve 4. Ventilation valve 5 tanks 6 Solvent tanks 7 Packers 8. Waste liquid tank 10 HPLC columns 11. Conveyor 21. Excess slurry 22 Transport Stocker 23. Trimming member 31 Column End 32 Mounting Unit 33 Holding part 34 Rotary power supply unit

Claims

1. An automatic column packing device for HPLC, which automatically fills the column with packing material, the device is A pressure supply device for controlling the output of pressure in the HPLC column automatic filling apparatus, A switching valve for adjusting the pressure inside the HPLC column automatic filling device, A vent valve for adjusting the pressure inside the HPLC column automatic packing device, which has been pressurized or depressurized, to atmospheric pressure, A tank for storing slurry containing packing material, One or more solvent tanks for storing the solvent, A packer is a container for storing the slurry containing the packing material supplied from the tank and the solvent tank by the pressure supply device, and for supplying the slurry to an HPLC column to fill it with the packing material. A waste liquid tank for recovering excess slurry and / or solvent that overflows from the HPLC column when the packing material is packed into the HPLC column, An automatic column packing apparatus for HPLC, characterized by comprising the following:

2. The HPLC column automatic filling apparatus according to claim 1, further comprising a conveyor having a function for attaching and / or detaching the HPLC column to the packer.

3. The HPLC column automatic filling apparatus according to claim 1, characterized in that the pressure supplied by the pressure supply device to the HPLC column automatic filling apparatus is 200 MPa or less.

4. The HPLC column automatic filling apparatus according to claim 1, further comprising a scraping member for scraping off excess slurry that has spilled out of the HPLC column after the packing material has been filled into the HPLC column.

5. The HPLC column automatic packing apparatus according to claim 4, characterized in that the leveling member is made of an elastic material or resin.

6. The HPLC column automatic filling apparatus according to any one of claims 1 to 5, further comprising a mounting unit for attaching a column end to the open end of the HPLC column after filling with the packing material.

7. The column end has a screw-in structure, The HPLC column automatic filling apparatus according to claim 6, characterized in that the mounting unit has a holding part for holding the column end and a rotational power supply part for rotating the holding part.

8. A method for automatically filling an HPLC column with packing material, wherein the method is: (a) A step of cleaning the piping and / or packers arranged in the HPLC column automatic packing device used in the method, (b) The step of attaching the HPLC column to a packer which functions as a container for filling the HPLC column with packing material, (c) A step of supplying a slurry containing a filler to the packer by controlling the pressure using a pressure supply device, (d) A step of supplying the slurry from the packer containing the slurry to the HPLC column by controlling the pressure using the pressure supply device, (e) The step of removing the HPLC column containing the packing material from the packer, including, A method characterized by the following:

9. The method according to 8, characterized in that in step (b) and / or step (e), the HPLC column is attached to and / or removed from the packer by using a conveyor.

10. The method according to the 8th method, characterized in that the pressure supplied by the pressure supply device to the HPLC column automatic filling device is 200 MPa or less.

11. The method according to 8, further comprising a step of scraping off excess slurry overflowing from the HPLC column between step (d) and step (e).

12. The method according to 11, characterized in that, in the step of scraping off the excess slurry, after the HPLC column is placed on the conveyor, the conveyor is moved so that it passes under the fixed scraping member, thereby scraping off the excess slurry.

13. The method according to 12, further comprising the step of attaching a column end to the open end of the HPLC column between the step of scraping off the excess slurry and step (e).

14. The method according to 13, characterized in that, in the step of attaching the column end, the column end having a screw-in structure is attached to the open end of the HPLC column by rotating and pushing it in.

15. An automatic column packing apparatus for HPLC used in the method according to any one of claims 8 to 14, wherein the apparatus automatically packs a packing material, A pressure supply device for controlling the pressure inside the HPLC column automatic filling apparatus, A switching valve for adjusting the pressure inside the HPLC column automatic filling device, A vent valve for adjusting the pressure inside the HPLC column automatic packing device, which has been pressurized or depressurized, to atmospheric pressure, A tank for storing slurry containing packing material, One or more solvent tanks for storing the solvent, A packer is a container for storing the slurry containing the packing material supplied from the tank and the solvent tank by the pressure supply device, and for supplying the slurry to an HPLC column to fill it with the packing material. A waste liquid tank for recovering excess slurry and / or solvent that overflows from the HPLC column when the packing material is packed into the HPLC column, An automatic column packing apparatus for HPLC, characterized by comprising the following:

16. The HPLC column automatic filling apparatus according to claim 15, further comprising a conveyor having a function for attaching and / or detaching the HPLC column to the packer.

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