JPS6273163A - Gas chromatograph apparatus - Google Patents

Abstract

PURPOSE:To dispense with a capillary tube as a resistance tube and to continuously change a split ratio, by supplying carrier gas to the inflow side of a capillary column to change the apparent resistance of a flow passage. CONSTITUTION:Carrier gas is supplied to a specimen injection port 3 and a pressure controller 7 in such a state that a four-way valve 6 was changed-over to the side of a capillary column 1. A specimen is carried by the carrier gas to reach a branch pipe 2 where receives the resistance of the pipeline of the capillary column 1 and the pressure of the carrier gas supplied through the pressure controller 7 to be divided by the flow dividing ratio determined by the ratio of both of them to flow to the side of the capillary column 1 and an atmosphere open flow passage consisting of a branch pipe 4 and a flow passage resistor 5. By this method, the specimen split to predetermined concn. by the operation of the pressure controller 7 is separated at every component by the capillary column 1 to be analyzed by a mass analyser 10.

Description

DETAILED DESCRIPTION OF THE INVENTION A. Field of Industrial Application The present invention relates to a gas chromatograph apparatus using a gear pillar column, and more particularly to a technique for adjusting a split ratio.

1. Prior Art For example, in a so-called gas chromatograph/mass spectrometer that uses a mass spectrometer as a component detection means, sample injection is necessary to prevent highly sensitive samples from flowing into the mass spectrometer. The inflow side of the column connected to the inlet is branched to connect a flow path resistance, and the split ratio is adjusted by manipulating this flow path resistance.

By the way, when a capillary column is used to separate the sample, it is possible to set the flow path resistance by preparing a large number of capillary tubes and adjusting the length of the capillary tubes according to the split ratio. It was being done. For this reason, there is a problem in that not only a large number of capillary tubes and connection mechanisms are required, but also the split ratio can only be set discretely.

C1 Purpose of the Invention In view of the above-mentioned problems, an object of the present invention is to provide a capillary column type gas chromatograph device that does not require a capillary tube as a resistance tube and can continuously change the split ratio. shall be.

The configuration of the twenty-nine invention, that is, the feature of the present invention is that carrier gas is supplied to the inflow side of the capillary column via a pressure regulating valve to change the apparent flow resistance.

E. Embodiments The details of the present invention will be explained below based on illustrated embodiments. FIG. 1 shows an embodiment of the present invention, in which reference numeral 1 denotes a capillary column, one end of which connects to a sample injection port 3 via a branch pipe 2, and the other end of which constitutes a detection section. The other end of the 6-minute end tube 2 connected to the mass spectrometer 10 is further shunted by a branch tube 4, one flow path is open to the atmosphere via a flow path resistance 5, and the other The flow path is connected to a four-way valve 6. This four-way valve 6 is connected to a flow path connected to a carrier gas source 12 via a pressure regulator 7 and a wave path connected to the pressure regulator 7 via a sealed container 9 containing a solvent 8. It is possible to select one of these wave paths.

Note that cylinder number 11 in Figure 1 indicates a receiver that accommodates the split sample.

In this embodiment, carrier gas is supplied to the sample injection port 3 and the pressure regulator 7 with the four-way valve 6 switched to the capillary column 1 side (flow path indicated by a solid line in the figure).

When such preparations are completed, a sample is injected from the sample injection port 3, and the sample is carried by the carrier gas and reaches the branch pipe 2.

The carrier gas containing the sample from the sample injection port 3 is subjected to the pipe resistance of the capillary column 1 and the pressure of the carrier gas supplied via the pressure regulator 7 in this branch pipe 2.
The flow is divided into the capillary column 1 side, the branch ¥-4, and the air-opening flow path consisting of the flow path resistance 5 according to the split flow ratio determined by the ratio of the two.

In other words, as the pressure of the carrier gas supplied from the pressure regulator 7 is lowered, the amount of sample diverted to the atmosphere open side gradually increases, and conversely, as the pressure is increased, the amount of sample is diverted to the capillary column 1 side. The number of samples to be analyzed gradually increases.

In this way, the sample is split to a predetermined concentration by operating the pressure regulator 7, and the components are separated by the capillary column 1 and analyzed by the mass spectrometer 10. On the other hand, the sample discharged to the atmosphere is condensed in the receiver 11 and the conduit leading thereto. When the injection of the sample is completed, the four-way switching valve 6 is switched to the other side (the flow path indicated by the dotted line in the figure), and the solvent 8 in the sealed container 9 is transferred to the branch pipe 4 using the carrier gas.
When the sample is poured into the pipe from the pipe to the receiver 11, the sample condensed in the pipe is dissolved and flows into the receiver 11, and the sample is recovered without waste.

In addition, a liquid such as a solvent is stored in the receiver 11 in advance, and the discharge end 1
By adjusting the liquid level relative to No. 3, it becomes possible to finely adjust the pipe resistance, that is, the tin lift ratio.

Although this embodiment has been described using a mass spectrometer as the detection means, it goes without saying that the same effect can be achieved when other detectors are used.

Effects As described above, according to the present invention, carrier gas is supplied via a pressure regulator in the middle of the pipe line leading from the sample injection port to the capillary column, and the pressure MA regulator is used. Not only is it possible to continuously adjust the amount of sample flowing into the capillary column through operation, but it also eliminates the need for a large number of capillary column tubes to form a resistance tube, reducing costs and downsizing the device. becomes possible.

[Brief explanation of drawings]

The figure is a configuration diagram of an apparatus showing an embodiment of the present invention. ■... Capillary column 2.4... Branch tube 3... Sample injection port 7... Pressure regulator 11... Receiver ■? ...Carrier gas source

Claims (1)

[Claims] A gas chromatograph apparatus in which a sample injection port and a capillary column are connected to a flow path open to the atmosphere via a branch pipe, and a carrier gas supply flow path via a pressure adjustment mechanism is connected in parallel to the branch pipe.