JPH08122314A - Gas-chromatography mass spectometric analyzer - Google Patents

Abstract

PURPOSE: To provide a gas-chromatography mass spectometric analyzer which can analyze a component in moisture without using a pretreatment apparatus. CONSTITUTION: A gas-chromatography mass spectrometric analyzer is provided with a gas chromatographic apparatus 10 and with a mass spectrometric analyzer 20. The gas chromatographic apparatus is provided with a precolumn 14 which is installed between an injector 10 and a main column 12 and which can separate moisture and with a valve by which a sample passed through the precolumn 14 can be sent to a flow passage on the side of the main column 12 and to a flow passage to the outside of a system so as to be changed over.

Description

Detailed Description of the Invention

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a gas chromatograph mass spectrometer, and more particularly to an apparatus for analyzing components in water.

[0002]

2. Description of the Related Art A mass spectrometer passes a particle sent from an ion source through an analysis field in a vacuum container maintained at a high vacuum to perform mass separation, and guides a particle having a desired mass to a detector. Is to detect. When the degree of vacuum in the mass spectrometric section drops, the ion particles cannot reach the detection section, which makes analysis impossible. Therefore, in the measurement of a sample containing water, it has become possible to analyze water components by adding various pretreatment devices to remove water or by expelling only the target component from water.

[0003]

In the gas chromatograph mass spectrometer, the gas chromatograph analyzer is connected to the preceding stage of the mass spectrometer. Conventionally, in such an analysis, the sample cannot be directly injected into the gas chromatograph mass spectrometer. It was not possible, and it took time to use the pretreatment device. In addition, the pretreatment device sometimes does not completely remove the moisture, and the moisture gradually enters the mass spectrometer, which causes background noise. Alternatively, a large-sized vacuum pump with a large exhaust capacity was required for the mass spectrometer. An object of the present invention is to solve the above problems and to provide a gas chromatograph mass spectrometer capable of directly introducing a sample containing water without using a pretreatment device.

[0004]

The gas chromatograph mass spectrometer of the present invention, which has been made to solve the above problems, has a gas chromatograph section for feeding and separating a sample injected from a sample inlet to a main column, and a gas chromatograph. In a gas chromatograph mass spectrometer having a mass spectrometer into which components separated by the main column of the tograph part are introduced, a pre-column that is provided between the sample introduction port and the main column and is capable of separating water, A valve that switches the destination of the sample that has passed through the precolumn to the main column side flow path and the flow path to the outside of the system, discharges the water separated by the precolumn to the outside of the system, and sends the target component to the main column It is characterized in that the components are separated by and are sent to the mass spectrometer.

The operation of this gas chromatograph mass spectrometer will be described below.

[0006]

In the gas chromatograph mass spectrometer of the present invention, the sample introduced from the sample inlet is separated from water and the target component by the precolumn provided in the gas chromatograph section. While water is being sent out from the pre-column, by switching the valve to the flow path connecting to the outside of the system, the water will be discharged out of the system and will not be sent to the main column and thereafter. By switching the valve to the main column side when water is not sent out from the pre-column, the target components other than water are introduced into the main column, separated into components, and sent to the mass spectrometer. Therefore, no water is sent to the mass spectrometer.

[0007]

Embodiments of the present invention will be described below with reference to the drawings. FIG. 1 is a block diagram of a gas chromatograph mass spectrometer showing one embodiment of the present invention.

In FIG. 1, 10 is a gas chromatograph, 20 is a mass spectrometer, and these are separators 30.
The flow path is connected via.

The inside of the gas chromatograph device 10 is mainly an injector 11 serving as a sample inlet and a main column 1.
2, consisting of a hexagonal valve 13 and a pre-column 14. The injector 11 is connected to an introduction path of He, which is a carrier gas, so that the sample introduced into the injector is sent to the valve 13 by He. The hexagonal valve has six ports from a to f. The port a is the injector 11, the port b is the inlet side of the precolumn 14, the port c is the supply source of He as a carrier gas, and the port d is the main column 12. , The port e is connected to the outlet side of the pre-column 14, and the port f is connected to the discharge path to the outside of the system. Then, by switching the valves, the first state in which af, bc, and de are connected,
A second state in which ab, cd, and ef are connected can be selected.

By switching the valve to the first state, the injector 11 is connected to the outside of the system through the port a and the port f, and the He supply source is the port c, the port b, the precolumn 14, the port e, the port d, the main. It is connected to the column 12.

By switching the valve to the second state, the injector 11, the port a, the port b, the pre-column 14, the port e, the port f and the discharge passage are connected,
The He supply source is connected to the port c, the port d, and the main column 12.

The outlet side of the main column 12 is a separator 3
0, the flow rate is adjusted in the separator 30, the sample component is sent to the mass separation unit 21 of the mass spectrometer 20, and is measured by the detection unit 22.

Next, the measurement operation of this apparatus will be described with reference to FIG. FIG. 2 shows the first state and the second state of the valve in order to explain the connection of the flow paths of the gas chromatograph apparatus of FIG.
FIG. 3 is an explanatory diagram showing the states separately and simplified.
2A corresponds to the second state, and FIG. 2B corresponds to the first state.
Here, for convenience, it is assumed that the water separated by the precolumn comes out earlier than the target component.

First, the sample is introduced from the injector 11 after switching to the second state shown in FIG. 2 (a). The introduced sample is sent to the pre-column 14 via the ab of the valve 13 by the carrier gas. In the pre-column 14, the water in the sample is separated from the target component, and the water first passes through. The water that has passed through the pre-column 14 is discharged to the outside of the system through the discharge passage between the ef of the valve 13. When the water is exhausted, the valve is switched to the first state shown in FIG. 2 (b). The target component remaining in the pre-column 14 passes through the pre-column 14 by the carrier gas and is sent to the main column 12 through the ed portion of the valve 13. And the main column 1
2 is separated into each component, and the separator 3 is separated for each component.
It is sent to the mass separation unit 21 of the mass spectrometer 20 via 0 and measured by the detector 22.

Since water is removed in advance, there is no water in this component, and the mass spectrometer 20 is not adversely affected by water.

Although a hexagonal valve is used in this embodiment, the valve is not limited to this. Moreover, the connection of the pipes is not limited to this. In short, when the water is released from the pre-column, it is connected to the discharge path connected to the outside of the system, and while the target component is released from the pre-column, it is connected to the main column. You may use piping.

Further, when a capillary column is used as the main column, a splitter may be provided between the valve and the main column to adjust the flow rate.

Further, by adjusting the temperature of the pre-column separately from that of the main column, it is possible to enable rapid water removal of the pre-column. Further, the back flush of the pre-column may be performed by using an eight-way valve or the like.

[0019]

As described above, according to the present invention,
A precolumn capable of separating water with a gas chromatograph mass spectrometer and a valve for switching the destination of the sample passing through the precolumn between the main column side flow path and the flow path to the outside of the system are provided, and the water separated by the precolumn is Since it was designed to be discharged out of the system and only the target component was sent to the main column, it is possible to analyze the components in the water without sending water to the mass spectrometer without using a pretreatment device. became.

[Brief description of drawings]

FIG. 1 is a configuration diagram of a gas chromatograph mass spectrometer according to an embodiment of the present invention.

FIG. 2 is an explanatory diagram for explaining the operation of the apparatus of FIG.

[Explanation of symbols]

 10: Vacuum container 11: Injector 12: Main column 13: Hexagonal valve 14: Pre-column 20: Mass spectrometer 30: Separator

Claims (1)

[Claims] 1. A gas chromatograph mass having a gas chromatograph section for sending a sample injected from a sample introduction port to a main column for separation, and a mass spectrometer for introducing a component separated by the main column of the gas chromatograph section. In the analyzer, a precolumn provided between the sample introduction port and the main column and capable of separating water,
A valve for switching the destination of the sample that has passed through the precolumn to the main column side flow passage and the flow passage to the outside of the system,
A gas chromatograph mass spectrometer, wherein the water separated by the pre-column is discharged to the outside of the system, and the target component is sent to the main column to separate the components and then sent to the mass spectrometer.