JPS5981556A - Cutting off device of sample introduction between chromatograph and succeeding analyzing equipment - Google Patents

Abstract

PURPOSE:To eliminate a blockaded space by a branched pipe line and to remove obstacles due to the residence of sample components by using the side of a main gas pipe line as a valve. CONSTITUTION:In case of introducing the flowing components out of a gas chromatograph G to a mass spectrometer M, a silica capillary K is inserted into the inner part of a nozzle (n) and an opening hole (b) is shut by the capillary K itself. A gas flowed out of the gas chromatograph G is jetted from the nozzle (n) and introduced to an orifice (f). When the sample introduction to the mass spectrometer is stopped, the tip end of the capillary K is retreated to the left side of the opening hole (b). The flowing gas out of the gas chromatograph is flowed from the opening hole (b) to a waste gas chamber C and is sucked and removed by a pump P. The problem that a part of the sample components is diffused and introduced into the blockaded space and flowed gradually to the succeeding analyzing equipment can be solved.

Description

DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a device for blocking gas flow between a gas chromatograph and another analytical device when the two are combined.

An analysis method is used in which a gas chromatograph is connected to another analytical device such as a mass spectrometer, and the sample components separated by the gas chromatograph are introduced into the mass spectrometer and then analyzed. .

In this case, a device for blocking gas flow is provided between the gas chromatograph and the analyzer connected thereto. Usually, this device is called a solvent diper, etc., and it not only collects the solvent of the sample flowing out from the gas chromatograph, but also collects the chromatograph effluent components that do not need to be analyzed in the subsequent analyzer. This is used for the inflow of W +4-, thereby preventing contamination of the subsequent analyzer with unnecessary components. The present invention relates to a gas flow conduction/blocking device provided between a gas chromatograph and an analysis device connected thereto for such purposes.

The conventional solvent diper has a tubing system T that connects the gas chromatograph O and another analyzer M, as shown in Fig. 11.
A branch pipe B is provided in the middle of
It is designed to be opened and sucked out. In this configuration, the pipe line from the branch point of the branch pipe B to the valve V and the space inside the valve are closed spaces, and the gas chroma I
・A part of the sample components flowing out from the graph expands into this closed space and gradually flows out toward the subsequent analyzer In device M, 7 is the peak with a tail.
There was a problem that the gas may be mixed with the next gas flow component (-) and a ghost may appear in the analysis results by the subsequent analyzer λ4.

The present invention has been made to solve the above-mentioned problems of conventional solvent dipers.

As shown in FIG. 2, the present invention connects a piping system connecting a gas chromatograph G and another analyzer M to a silica capillary extending from a gas chromatograph (club) and a sample sample extending from a subsequent analyzer M. The inner diameter of the open end of the pipe is set so that the outer diameter of the pipe can be inserted so that the outer diameter of the pipe is suitable for insertion, and the side opening is was installed and connected to the exhaust system Q, and the side opening was opened and closed by inserting the silica capillary K from the open end of the pipework to the depth of the opening marked L, or stopping it before the opening marked B. The present invention utilizes the flexibility, high mechanical stability, and heat resistance of a silica capillary to enable the above-mentioned configuration (which will be implemented below). The invention will be explained by way of example.

FIG. 3 shows a main part of an embodiment of the present invention. This embodiment combines a gas chromatograph and a mass spectrometer and relates to an apparatus. When combining a gas chromatograph and a mass spectrometer, a molecular separator is used to remove the carrier gas from the gas chromatograph outflow gas and concentrate the sample components before introducing them into the mass spectrometer.

A pallet is used. In FIG. 3, S is a molecular separator and a jet type molecular separator is used. The jet-type molecular separator has a nozzle n and an orifice f facing each other in an exhaust chamber C, and a force λ chromatograph G is applied to the nozzle n.
Connect the orifice to analyzer M. This nozzle part is a pipe system extending from the analytical cutter 111, and is inserted into the silica capillary IJK extending from the gas chromatograph G or nozzle 1]. The nozzle n is provided with openings r and lb on the d side, and these openings open into the exhaust chamber C, and the exhaust chamber C is connected to the vacuum pump P.
Therefore, the exhaust chamber corresponds to a part of the exhaust system Q mentioned above.

When introducing the gas chromatograph effluent component into the mass spectrometer with the above configuration, the silica capillary K is connected to nozzle n.
At the age of nine, he entered the capillary and opened it himself []1]
block. In this way, the gas flowing out from the gas chromatograph is ejected from the nozzle n, and at this time, the light carrier gas molecules d such as helium, 47E K+, are larger than the molecules of the sample component to the side of the orifice. The concentration of the 12-sample 1 component is significantly increased in the gas entering the gas. When stopping sample introduction to the quality fi analyzer, move the tip of the cabin IJK back with the left side handle of the opening. This opens the opening nb, and the gas chromatograph outflow immediately flows into the exhaust chamber C and is removed by suction by the pump P. In this case, since the opening of the nozzle n has a large outflow resistance, most of the chromatograph outflow gas flows out and is removed. In addition, since the pressure inside nozzle n has decreased, even if a portion of the chromatograph outflow gas flows out from nozzle n, no jet can be formed and nozzle n
and orifice f, and cannot enter the mass spectrometer.

Airtightness between the silica capillary and the nozzle n is achieved by a compatible fit between the two, and no lubricant is used. If pure carrier gas is introduced near the capillary insertion end of nozzle n, the carrier gas will flow out from the capillary insertion end of the nozzle and prevent outside air from entering. The fit between the capillary and the capillary can be quite loose. Of course, a backing may be used between the nozzle n and the + tip. FIG. 4 shows another embodiment of the present invention in which the silica gear pillar K extended from the gas chromatograph G is extended from the nozzle of the molecular sehaleke S. An opening is provided on the side of the inflow pipe Vζ (~, L') into the nozzle and connected to the chaste pump P, and its usage is the same as the example shown in FIG. 3 above.

The device of the present invention has the above-mentioned configuration, and there is no branch pipe as in the conventional example, and the side of the main gas pipe is used as a valve, so a closed space is not formed as in the conventional example. Various problems caused by retention of sample components are all eliminated.

[Brief explanation of drawings]

FIG. 1 is a side view of a conventional example, FIG. 2 is a side view showing the general configuration of the present invention, FIG. 3 is a vertical side view of one embodiment of the present invention, and FIG. 4 is another embodiment of the present invention. It is a longitudinal side view of an example. Q...Gas chromatograph, M...Other analytical equipment, K
...silica gear pillar extending from the gas chromatograph, L...sample introduction tubing extending from the analyzer M, b...side opening of the tubing, Q...opening 1]
Exhaust system connected to.

Claims (1)

[Claims] A silica capillary extended from the column of the Kass chromatograph is slidably inserted into the open end of the sample introduction tube system of another analyzer connected to the Kass chromatograph (-1) The capillary insertion part of the test tube introduction tube system Open "1" on the side of
A chromatograph characterized in that the opening is opened or closed by adjusting the depth of insertion of the silica capillary into the sample introduction pipe system, or is closed with the white of the silica capillary. Sample introduction cut-off device between the and the subsequent analyzer.