JPS62130355A - Preparative gas chromatography - Google Patents

Abstract

PURPOSE:To assure a flow passage selection function regardless of a column sepn. temp. so that the separated components are taken by connecting the outlet of a flow rate branching part, component capturing devices and the inlet of the flow rate branching part in a manner as to correspond the same one to one and taking the components separated by the column successively into the component capturing devices by selecting the flow passage selection part. CONSTITUTION:The flow passage branching part 8 is provided in a thermostatic chamber 1 and a flow passage selector valve 10 for selecting the flow passages for the gases passing through the branching part 8 is installed on the outside of the chamber 1 and behind the component capturing device 9. A trap using liquid nitrogen, etc. as a coolant is used for the device 9 according to the components to be taken. The sample is then introduced from a sample introducing part 2 and is separated 3 to the respective components. A conduit piping of carrier gas to be let out of a detecting part 4 is branched 8 and is captured 9 via the branch pipe 8-1 until the intended component is detected in the part 4. The conduits are so selected 10 in this stage that the conduit led out of the device 9 is held open and that the conduit led out of the device 9' for capturing the intended component is held closed. The intended 10 is captured 9 by the selection 10 when the separation of the intended component is detected.

Description

[Detailed Description of the Invention] [Industrial Application Field] The present invention relates to a preparative gas chromatograph device, and particularly to a preparative gas chromatograph device that performs a preparative separation operation at a column separation temperature that is higher than the heat resistance temperature of a switching valve that switches the flow path of a component to be separated. The present invention relates to a preparative gas chromatograph device that can perform a preparative gas chromatography.

[Conventional technology]

A conventional preparative gas chromatograph apparatus is shown in FIG. A sample injection section 2, a separation column 5, a detection section 4, a control column 6 in some cases, and a flow path switching valve 10 are housed in a thermostatic chamber 1, and a component collector 9 is provided outside the thermostatic chamber 1. The sample introduced from the sample injection part 2 is accompanied by the carrier gas introduced through the sample/carrier gas dedicated pipe 5VC, and is passed through the separation column 5VC.
It is sent, separated into components, and then sent to the detection section 4,
In case z! After being compared with the carrier gas introduced through the pipe 7 and the control column 6 in the detection section 4, the carrier gas 4 is separated into the component collector 9 or discharged as necessary in the flow path switching valve 10. is being manipulated.

[Problem that the invention seeks to solve]

The inside of the constant temperature chamber is maintained at the column separation temperature, so if this temperature is higher than the heat resistance of the flow path switching valve, the chamber will cause gas leakage or seizure, and the flow path switching function will be lost. However, foolproof operation of the gas chromatograph cannot be guaranteed.

[Means for solving problems]

The present invention eliminates the drawbacks of conventional preparative gas chromatograph devices as described above, ensures flow path switching function regardless of column separation @ degree, and enables preparative fractionation of separated components. The purpose of this device is to provide a gas chromatograph device, which has a sample injection part, a separation column, a detection part, and a flow path branch part inside a thermostatic chamber, and a separation section for separation and collection outside the thermostatic chamber. A number of component collectors and flow path switches S corresponding to the number of strokes are provided, and these are connected in the above order with a carrier gas conduit. match the number of component collectors,
The outlet of the flow path branch part, the component collector, and the flow path switching function port are connected to one another.
This is achieved by constructing a preparative gas chromatograph apparatus, which is characterized in that the components are connected in correspondence with each other, and the components separated by the Ericolumn can be sequentially collected by the component collector by switching the flow path switching section.

[For production]

FIG. 1 is a conceptual diagram showing an example of the apparatus of the present invention. In the apparatus of the present invention, a flow path branching section 8 is provided inside the thermostatic chamber 1, and a flow path switching valve 10 for operating the switching of the flow path of gas passing through the flow path branching section is provided outside the thermostatic chamber as a component collector. Installed behind 9. As a component collector, a trap using liquid nitrogen, dry ice, or ice as a cooling agent is used depending on the component to be separated.

In order to separate and recover one target component using the apparatus of the present invention, a sample is introduced into the sample injection section 2, and the sample is separated into each component in the separation column 3. At 1, when the target component is detected in the detecting section 4, the carrier gas conduit led out from the detecting section 4 is branched at the flow path branching section 8, and collected in the fraction collection path 9 through the branching path 8-1. At this time, the flow path switching valve is positioned to open the conduit leading out from the component collector 9 and close the conduit leading out from the component collector 9' that collects the target component. When separation of the target component is detected, the flow path switching valve 10 is switched to open the conduit leading out from the component collector 9'' that collects the target fraction,
Leave it in a free state. The target component passes through the branch path 8-2 at the flow path branch section 8 and is collected by the component collector 9'.

In addition, although FIG. 1 shows a diagram in which one component collector is installed to collect target components and non-target components, the number of branch channels and It is also possible to increase the number of component collectors and the number of inlets of flow path switching valves. (Refer to Figures 5 to 8) In this case, the flow path switching valve 10 may be used in combination with two-way switching valves as shown in Figures 5 and 6 to separate and recover multiple components separately. A multi-way switch having an inlet individually corresponding to each conduit leading out from the component collector may be provided. In either case, the flow path switching valve 10 closes the other conduit when at least one conduit is opened. It is configured as follows.

In addition, in the bag #LVc of the present invention, a carrier gas introduction W7 is connected to the flow path branching part 8 shown in FIG. In addition, it is also possible to prevent unintended components from being introduced into the portion 8. That is, while the unintended components are flowing out, the flow path switching valve is set to the negative state (FIG. 3), and the unintended components are collected in the component collector 9.

At this time, the carrier gas is introduced from behind the branch path 8-1 through which the unintended fraction is led out at the flow path branch section 8 through the carrier gas introduction pipe 7 and the resistance column 1). At this time, the flow of the gas is as shown in FIG. 4(a), and the carrier gas introduced from the carrier gas introduction t7 diffuses into the branch path 8-2 where the unintended fraction leads out the target component. to prevent When the target component flows out through the separation force Ramef and is detected by the detector, the flow path switching valve 10 is set to the state shown in FIG. 3(1)), and the target fraction is collected in the component collector 9'. The gas flow at this time is as shown in FIG. 4 (1)), and the target component is led out through the branch path 8-2. In this method, in the flow path switching section 8, if the carrier gas introduction pipe is connected to the rear of the branch path 8-1 which leads out the unintended fraction and to the front of the branch path 8-2 which leads out the target component, the unintended component can be removed. This can prevent contamination with ingredients.

Note that if the on-off valve is switched to the direction that collects the target component immediately after the outflow of the target component is detected, unintended components may remain in the flow path switching section and may mix with the target component. Therefore, by switching the flow path in consideration of the delay from the detector to the component collector, it is possible to prevent the target component from being contaminated with the non-target component.

Alternatively, instead of providing the resistance column 1), a capillary or a carrier gas introduction pipe is guided outside the tank as shown by the dotted line in Figure 2, and a flow rate adjustment device 12 is connected to this introduction pipe outside the tank.
may be connected.

Furthermore, the case of separating multiple target fractions is shown in Figures 5 to 8.
As shown in the figure. Although the figure shows an example in which three component collectors are provided, the number can be increased according to the number of fractions.

In FIGS. 5 and 7, the flow path branching portion 8 is composed of one main flow path and a plurality of branch paths 8-1, 8-2, and one branch path is formed at one location. The carrier gas passing through the resistor column 1) can be introduced into the branch part by introducing it slightly behind the last branch in Fig. 5, or from 7' in Fig. 6; There are some that are introduced from the rear 7' and 7'. By switching the flow path at a rate of 10.10', the components flowing out from the separation column are sequentially transferred to the component collector 9. as shown in FIGS. 6(a) to (C). 9', 9' can be collected. Figure 7 is a modification of the method of introducing carrier gas at each branch in Figure 5, in which carrier gas is introduced into pJr near the branch point of each branch path, and like the method of Figure 2, other components Contamination can be prevented.

Further, in FIG. 8, the conduit from the detector 4 is divided into branch paths of the same number as the number of fractions at one point. Then, carrier residue is introduced into each branch path slightly downstream from the branch point to prevent other components from being mixed in.

〔Effect of the invention〕

By employing the above configuration, the present invention enables gas chromatography operation at a column separation temperature higher than the column separation temperature, which is higher than the heat resistance temperature of the switching valve that switches the flow path of the fraction to be fractionated. By connecting a carrier gas introduction pipe to a specific part of the TFC channel branch, it is also possible to separate the target component without mixing other components.

[Brief explanation of drawings]

Figures 1, 2, 5, 7 and 8 are conceptual diagrams of an example of the apparatus of the present invention;
a), (b) are diagrams showing the gas flow and the state of the flow path switching valve in the flow path switching section and flow path branching section of the device shown in FIG. 2, FIGS. 6 (a), (t)), (C-) is a diagram showing the state of the flow path for preparative fractionation at the flow path switching section and flow path branching section of the device shown in FIG. 5, and FIG. 9 is a conceptual diagram of a conventional preparative gas chromatograph device. be. DESCRIPTION OF SYMBOLS 1... Constant temperature chamber, 2... Sample injection part, 3... Separation column, 4... Detection part, 8... Channel branch part, 9, 9
', ? '・'...Component collector, 10...Flow path switching valve

Claims (7)

[Claims] (1) A sample injection section, a separation column, a detection section, and a flow path branching section are installed inside the constant temperature chamber, and a number of component collectors and flow path switching sections corresponding to the number of fractions of components to be separated and recovered are installed outside the constant temperature chamber. and connect them in the above order with a carrier gas conduit,
At that time, the number of outlets of the flow path branching section and the number of inlets of the flow path switching section are made to match the number of component collectors, and the number of exits of the flow path branching section, component collectors, and inlets of the flow path switching section is set to one. Connect them one by one,
1. A preparative gas chromatograph apparatus characterized in that components separated in a column can be sequentially collected into a component collector by switching a flow path switching section. (2) The flow path branch part consists of one main flow path and multiple branch paths, forming one branch path at one location with respect to the main flow path, and introducing carrier gas slightly behind the last branch or each branch. The preparative gas chromatograph apparatus according to claim 1, characterized in that a pipe is connected to the preparative gas chromatograph apparatus. (3) A patent claim characterized in that the flow path branch part consists of one introduction path and a plurality of branch paths, and a carrier gas introduction pipe is connected to each branch path slightly behind each branch path. The preparative gas chromatograph apparatus according to item 1. (4) A resistance column is provided in the constant temperature chamber, and this is connected to the carrier gas introduction pipe at the flow path branch, so that the carrier gas can be introduced into the component collector together with the separation column outflow gas. A preparative gas chromatograph apparatus according to claim 2 or 3, characterized in that: (5) The preparative gas chromatograph apparatus according to claim 2 or 5, characterized in that a flow rate control valve is provided in the carrier gas introduction pipe of the flow path branching section. (6) A patent characterized in that the flow path switching section is formed by combining a plurality of two-way switching valves to form the same number of inlets as the component collectors, and conduction can be made by selecting one of the component collectors. A preparative gas chromatograph apparatus according to any one of claims 1 to 5. (7) A patent claim characterized in that the flow path switching section is a multi-way switching valve, each component collector is connected to an inlet of the switching valve, and one of the component collectors is selected to be conductive. The preparative gas chromatograph apparatus according to any one of the ranges 1 to 5.