WO2017017765A1

WO2017017765A1 - Automatic tube connection device

Info

Publication number: WO2017017765A1
Application number: PCT/JP2015/071262
Authority: WO
Inventors: 努大古場
Original assignee: 株式会社島津製作所
Priority date: 2015-07-27
Filing date: 2015-07-27
Publication date: 2017-02-02
Also published as: JP6516010B2; JPWO2017017765A1

Abstract

This automatic tube connection device is provided with a pressure sensor for detecting the pressure inside a fluid feeding tube, a pressure state determination unit for determining whether the inside of the fluid feeding tube is pressurized on the basis of a detection value from the pressure sensor, and a control unit configured so as to prevent a needle from separating from a container member when the inside of the fluid feeding tube is pressurized.

Description

Automatic pipe connection device

The present invention provides an automatic pipe that automatically connects pipes to a container member such as an analysis column, a trap column, and an extraction container through which a fluid is passed in a liquid chromatograph or a supercritical fluid chromatograph using a needle seal structure. The present invention relates to a connection device.

There is a needle seal structure as a structure for connecting pipes easily and quickly. With the needle seal structure, the needle provided at the tip of the pipe is inserted into the opening provided in the object to be connected, so that the inner peripheral surface of the opening and the outer peripheral surface of the needle tip are in line contact and the pipe is to be connected. It is a structure that is connected to an object while maintaining liquid tightness. The needle seal structure is used for an injection port in an autosampler of a liquid chromatograph, for example.

For example, Patent Document 1 proposes that the extraction container can be easily attached to and detached from the apparatus by connecting the pipe to the extraction container of the supercritical fluid component extraction apparatus using the above needle seal structure. In addition, a plurality of extraction containers are installed in the apparatus, and movable needles are connected to these extraction containers by a needle seal structure, so that piping connection to the extraction containers to be used is automatically performed by moving the needles. It is also proposed to change it.

JP 2014-160055 A

If the needle seal structure is used, not only the piping connection to the extraction container in the supercritical fluid component extraction apparatus but also the piping connection to the analysis column or trap column in the liquid chromatograph can be automatically performed. With a liquid chromatograph or a supercritical fluid component extraction device, the residual pressure does not release immediately even after the mobile phase liquid supply is stopped, and immediately after the mobile phase liquid supply is stopped, the pipe connection needle is connected to a column, etc. When the container member is separated from the container member, there is a problem that the liquid is ejected from the needle tip or the opening of the container member. This is particularly noticeable when a mobile phase having a high compression rate is used.

In order to solve the above problem, a fixed time is set as a “depressurization time” for decreasing the residual pressure after the mobile phase liquid supply is stopped, and the needle is moved after the fixed time has elapsed. It is conceivable to take a method of pulling out from the container member. However, since the actual residual pressure varies depending on the flow rate of the liquid and the type of mobile phase, if the pressure release time is set short, the needle is not sufficiently reduced until the residual pressure is sufficiently reduced due to insufficient pressure release time. Will be pulled out and liquid will be ejected. Therefore, it is necessary to set the pressure release time longer than necessary.

When analyzing with a liquid chromatograph or supercritical fluid chromatograph, there is a need to reduce the time required for analysis as much as possible, but as described above, when the pressure release time until the needle is pulled out from the container member is longer than necessary Therefore, the time required for the analysis becomes longer accordingly.

Therefore, an object of the present invention is to optimize the timing for detaching the pipe from the container member in an automatic pipe connecting device that attaches / detaches the pipe to / from the container member by the needle seal structure.

One embodiment of an automatic pipe connecting device according to the present invention includes a fluid feeding pipe for feeding a fluid, a needle provided at one end of the fluid feeding pipe, and a fluid feeding by inserting the needle. A needle seal structure that allows fluid communication between the pipe and the internal space is provided at one end, and a needle for connecting or disconnecting the needle to the container member and a container member that allows fluid to flow in the internal space. A needle drive mechanism for moving the pressure sensor, a pressure sensor for detecting the pressure in the fluid feed pipe, and a pressure state determination unit for judging whether or not the fluid feed pipe is in a pressurized state based on a detection value of the pressure sensor; A control unit configured to control the operation of the needle drive mechanism, and based on the determination result of the pressure state determination unit, the needle is not detached from the container member when the fluid feeding pipe is in a pressurized state; It includes those were.
Here, “the inside of the fluid delivery pipe is in a pressurized state” means that the pressure in the fluid delivery pipe is higher than the atmospheric pressure.

In one embodiment of the automatic pipe connection device according to the present invention, a pressure sensor for detecting the pressure in the fluid feed pipe, and whether or not the fluid feed pipe is in a pressurized state based on the detection value of the pressure sensor. When the inside of the fluid feeding pipe is in a pressurized state, the pressure state judging unit that performs the control and the controller configured to prevent the needle from being detached from the container member when the inside of the fluid feeding pipe is in a pressurized state are provided. Thus, the needle is not detached from the container member, and the liquid can be prevented from being ejected from the needle tip or the opening of the container member. And since the pressure state in the fluid delivery pipe can be monitored, the needle can be detached from the container member at an appropriate timing without waiting for the needle for an unnecessarily long time after stopping the delivery of the mobile phase. It becomes possible to shorten the time required for analysis.

It is a flow-path block diagram which shows roughly one Example of the concentrated liquid chromatograph provided with the automatic piping connection apparatus. It is a section lineblock diagram showing roughly the column connection device (automatic pipe connection device) in the example. It is a block diagram which shows the structure of the Example schematically. It is a flowchart which shows an example of operation | movement of the Example. It is a graph which shows an example of the time change of the detection pressure of a pressure sensor. It is a flow-path block diagram which shows the state at the time of sample concentration in the Example. It is a flow-path block diagram which shows the state at the time of the analysis in the Example.

As a pressure state determination unit in the automatic pipe connection device of the present invention, when the output signal of the pressure sensor exceeds a preset threshold value, it is determined that the inside of the fluid feeding pipe is in a pressurized state. What is comprised is mentioned.

In the automatic pipe connection device of the present invention, a plurality of container members are provided, and the control unit is configured to connect the needle to one container member selected from the plurality of container members. Is preferred. Then, the container member to be used can be automatically changed by moving the needle.

An example of a liquid chromatograph having an automatic pipe connection device will be described with reference to the drawings. First, the flow channel configuration of this embodiment will be described with reference to FIG.

In this embodiment, a sample is once captured in a trap column and concentrated, and then the concentrated sample is guided to an analysis column for separation analysis. An autosampler 4 for injecting a sample is provided on the mobile phase liquid flow path 6 for concentration. The concentration mobile phase feeding flow path 6 is a path through which the concentration mobile phase is fed by the liquid feed pump 2. The concentration mobile phase liquid flow path 6 is connected to one of the ports provided in the rotary high pressure valve 8.

The high pressure valve 8 is a two-position valve having six ports and switching the connection between adjacent ports. Each port of the high-pressure valve 8 includes a concentration mobile phase liquid flow path 6, a drain, a column inlet flow path 10, a column outlet flow path 14, an analysis mobile phase liquid flow path 18 and an analysis flow path 20. It is connected.

The high-pressure valve 8 is provided between the concentration mobile phase liquid flow path 6 and the column inlet flow path 10, between the column outlet flow path 14 and the drain, and to the analysis mobile phase liquid flow path 18 and the analysis flow path 20. (The state shown in FIG. 6; hereinafter referred to as the concentration mode), between the concentration mobile phase liquid flow path 6 and the drain, between the column inlet flow path 10 and the analysis mobile phase liquid supply. One of a state (a state shown in FIG. 7, hereinafter referred to as an analysis mode) in which the channel 18 is connected and the column outlet channel 14 and the analysis channel 20 are connected.

The column inlet channel 10 is connected to the inlet 39 (see FIG. 2) of the column connecting device 12 (automatic pipe connecting device), and the column outlet channel 14 is connected to the outlet 52 (see FIG. 2) of the column connecting device 12. Has been. Although the column connection device 12 will be described later, a trap column for concentrating the sample is accommodated in the column connection device 12.

The mobile phase feeding flow path for analysis 18 is a flow path through which the mobile phase fed by the mobile phase feeding apparatus 16 flows. The mobile phase liquid feeding device 16 includes

liquid feeding pumps

16a and 16b for feeding different solvents, and a mixer 16c for mixing the solvents fed by the

liquid feeding pumps

16a and 16b.

On the analysis flow path 20, there are provided an analysis column 22 for separating a sample for each component, and a detector 24 for detecting the sample component separated by the analysis column 22.

The column connection device 12 will be described with reference to FIG.

The inlet 39 and the outlet 52 are provided in the casing of the column connection device 12. The column inlet channel 10 is connected to the inlet 39, and the column outlet channel 14 is connected to the outlet 52. The inlet 39 is connected to the upper needle 38 via a pipe 40 (fluid feed pipe). The upper needle 38 is moved by the needle drive mechanism 44 in the horizontal plane direction and the vertical direction with the tip thereof directed vertically downward.

A plurality of lower needles 28 are provided at a position below the upper needle 38. The lower needle 28 is supported by a support table 30 with the tip thereof facing vertically upward. Each lower needle 28 is connected to a port of a rotary column selection valve 46 through a flow path 45. The column selection valve 46 has a common port at the center, and an outlet channel 50 leading to the outlet 52 is connected to the common port. The column selection valve 46 selectively switches and connects any one of the lower needles 28 to the outlet channel 50 by rotating the rotor provided with the channel 48.

A trap column 32 (container member) is installed above each lower needle 28. The trap column 32 is installed on the lower needle 28 while being held by the rack 31.

Needle seal structures

34 and 36 are provided at the lower end and the upper end of each trap column 32, respectively. The needle seal structure is an opening that communicates with the internal space. By inserting the needle tip into the opening, the needle seal structure is in line contact with the outer peripheral surface of the needle tip so that the inner space and the inner flow path of the needle are kept liquid-tight. It is a structure that allows communication.

The tip of the lower needle 28 is inserted and connected to the needle seal structure 34 at the lower end of each trap column 32. The needle seal structure 36 at the upper end of each trap column 32 is for inserting and connecting the upper needle 38.

A pressure sensor 42 is provided on the proximal end side of the upper needle 38. The pressure sensor 42 detects the pressure in the pipe 40. The pressure value detected by the pressure sensor 42 is taken into the control device 56 via the control unit 54 described later (see FIG. 3).

The configuration of the entire liquid chromatograph will be described with reference to FIG.

The concentration feeding pump 2, the analysis feeding device 16, the autosampler 4, the high pressure valve 8 and the column exchange device 12 are connected to a common control device 56. The control device 56 is realized by, for example, a general-purpose personal computer or a dedicated computer. The column connection device 12 is provided with a control unit 54 that controls the operation of the needle drive mechanism 44 and the column selection valve 46. The control unit 54 is a computer dedicated to the column connection device 12. The detection signal of the pressure sensor 42 is taken into the control device 56 via the control unit 54.

The control device 56 includes an analysis operation management unit 58, a pressure state determination unit 60, and a threshold value holding unit 62. The analysis operation management unit 58 manages the operations of the concentration liquid delivery pump 2, the analysis liquid delivery device 16, the autosampler 4, the high-pressure valve 8, and the column exchange device 12 so that a series of analysis operations to be described later is executed. Is. The pressure state determination unit 60 applies the pressure in the pipe 40 when the upper needle 38 is connected to one of the trap columns 32 by comparing the output signal of the pressure sensor 42 with a preset threshold value. It is comprised so that it may determine whether it is a pressure state. The threshold value used by the pressure state determination unit 60 is set based on, for example, the atmospheric pressure measured in advance. The set threshold value is held in the threshold value holding unit 62. When the output signal of the pressure sensor 42 exceeds the threshold value, the pressure state determination unit 60 determines that the inside of the pipe 40 is in a pressurized state.

Next, an example of the operation of this embodiment will be described with reference to the flowchart of FIG. 4 together with FIG. 2, FIG. 6 and FIG.

First, in the column connection device 12, the upper needle 38 is connected to the trap column 32 to be used, the high-pressure valve 8 is set to the concentration mode, and the feeding of the concentration mobile phase is started (see FIG. 6). Then, the sample is injected into the concentration mobile phase liquid flow path 6 by the autosampler 4, and the sample is captured by the trap column 32.

After the sample is captured in the trap column 32, the high pressure valve 8 is set to the sample introduction mode, the analysis mobile phase is fed by the analysis mobile phase feeding device 16, and the sample is introduced into the analysis channel 20 (FIG. 7). reference.). As a result, the sample captured by the trap column 32 is guided to the analysis column 22 and separated for each component. Sample components separated by the analysis column 22 are detected by a detector 24.

After the analysis of the sample is completed, the mobile phase liquid feeding by the analysis mobile phase liquid feeding device 16 is stopped. Immediately after stopping the mobile phase liquid feeding, the trap column 32, the upper needle 38, and the inside of the pipe 40 are pressurized by the residual pressure. If the upper needle 38 is detached from the trap column 32 in this state, there is a problem that liquid is ejected from the tip of the upper needle 38 or the opening of the needle seal structure 36 at the upper end of the trap column 32 and the inside of the apparatus is contaminated. is there.

Therefore, in this embodiment, the pressure in the pipe 40 is monitored by the pressure sensor 42 so that the upper needle 38 is not detached from the trap column 32 when the inside of the pipe 40 is in a pressurized state. Whether or not the pressure in the pipe 40 is in a pressurized state is determined by comparing the output value of the pressure sensor 42 with a preset threshold value.

FIG. 5 is a graph showing an example of the time change of the pressure in the pipe 40 detected by the pressure sensor 40. As shown in this graph, there is a residual pressure in the pipe 40 immediately after the mobile phase liquid feeding is stopped, and the residual pressure decreases with time. Then, when the output value of the pressure sensor 40 becomes equal to or less than a threshold value (for example, atmospheric pressure + 10%) set based on the atmospheric pressure, the upper needle 38 is separated from the trap column 32, whereby the inside of the pipe 40 is It drops to atmospheric pressure. Thereby, the ejection of the liquid from the tip of the needle 38 or the trap column 32 can be prevented.

In the above embodiment, the automatic pipe connection device is applied to a concentrated liquid chromatograph. However, the automatic pipe connection device of the present invention includes a plurality of extraction containers in a supercritical fluid extraction apparatus, and the extraction container to be used is needle-sealed. It can also be applied as a device that automatically changes depending on the pipe connection by structure. Further, the present invention can also be applied as a device that includes a plurality of analysis columns used for separating a sample of a liquid chromatograph and that changes the analysis column used by pipe connection with a needle seal structure.

2 Mobile phase feeding pump for concentration 4 Autosampler 6 Mobile phase feeding flow path for concentration 8 High pressure valve 10 Column inlet flow path 12 Column connection device (automatic pipe connection device)
14 Column outlet flow path 16 Analytical mobile phase liquid feeding device 18 Analytical mobile phase liquid flow path 20 Analytical flow path 22 Analysis column 24 Detector 28 Lower needle 30 Support table 31 Rack 32 Trap column (container member)
34, 36 Needle seal structure 38 Upper needle 39 Inlet part 40 Piping (fluid feed pipe)
42 Pressure sensor 44 Needle drive mechanism 46 Column selection valve 50 Outlet flow path 52 Outlet part 54 Control part 56 Control device 58 Analysis operation management part 60 Pressure state determination part 62 Threshold holding part

Claims

A fluid delivery pipe for delivering fluid;
A needle provided at one end of the fluid feed pipe;
A container member that has a needle seal structure at one end to allow fluid communication between the fluid feeding pipe and the internal space by inserting the needle and maintaining fluid tightness;
A needle drive mechanism for moving the needle to connect or disconnect the needle to or from the container member;
A pressure sensor for detecting the pressure in the fluid feed pipe;
A pressure state determination unit that determines whether or not the inside of the fluid feeding pipe is in a pressurized state based on a detection value of the pressure sensor;
A control unit configured to control the operation of the needle driving mechanism and based on the determination result of the pressure state determination unit, so that the needle is not detached from the container member when the fluid feeding pipe is in a pressurized state. And an automatic pipe connecting device.
The pressure state determination unit is configured to determine that the fluid feeding pipe is in a pressurized state when an output signal of the pressure sensor exceeds a preset threshold value. 1. The automatic pipe connection device according to 1.
A plurality of the container members;
The automatic pipe connection device according to claim 1 or 2, wherein the control unit is configured to connect the needle to one container member selected from the plurality of container members.