JPS60149969A - Column connection apparatus of gas chromatography apparatus - Google Patents

Abstract

PURPOSE:To make it possible to perform the exchange of a column in an evacuated state without sucking dust, by connecting a gas supply pipe, which supplies exchanging gas to the inlet part of a separator when the column is exchanged, to a connection member. CONSTITUTION:When the handle 10d of a change-over valve 10 is rotated to change over a flowline to an exchange mode terminal 10b, exchanging gas such as air is supplied from a supply source 13 through a constant pressure valve 12 and enters the connection pipe 4a of a connection member 4 from the valve 10 through a gas supply pipe 9 while dust therein is removed by a filter 11 and supplied to the inlet part 5a of a separator. The nut 4d of a connection member 4 is detached, while evacuation is succeeded from an exhaust pipe 5c in this state, to exchange a column and the nut 4d is clamped to complete the exchange of the column. If analysis is performed in this state after the column is exchanged the tailing phenomenon of a solvent and specimen due to te dead volume of the pipe 9 is generated and, therefore, the flowline of the valve 10 is changed over to an analytical mode terminal 10c and the analytical carrier gas in the pipe 9 is introduced to be substitute with the previous exchanging gas.

Description

DETAILED DESCRIPTION OF THE INVENTION [Technical Field of the Invention] The present invention relates to a device for connecting a column outlet and a separator inlet of a gas chromatography apparatus.

[Prior art]

FIG. 1 is a sectional view showing a conventional gas chromatography mass spectrometer, and FIG. 2 is a sectional view of its separator.

In the drawing, reference numeral 1 denotes a back column for gas chromatography, which is installed in a gas chromatography oven 2. The backed column 1 is filled with a packing material for sample development, and its column inlet 1a is connected to the sample vaporization section 3, and its column outlet 1b is connected to the separator inlet 5a of the separator 5 through a connecting member 4. ing. A carrier gas introduction pipe 6 is connected to the sample vaporization section 3 . The separator 5 has a structure in which an exhaust pipe 5c is connected to opposing parts of a separator inlet part 5a and a separator outlet part 5b, and is provided in a separator oven 5d. The other end of the separator outlet portion 5b is connected to an ion source chamber 8 provided in the ion source 7 of the mass spectrometer, and the exhaust pipe 5c is connected to an exhaust pump (not shown).

In the above configuration, a sample introduced into the sample vaporization section 3 by a microsyringe (not shown) is vaporized, and is sent to the back column 1 and developed by the carrier gas introduced from the carrier gas introduction tube 6. The developed sample and carrier gas enter the separator inlet 5a from the column outlet 1b via the connecting member 4. In the separator 5, the carrier gas among the gases blown out from the separator inlet 5a is discharged from the exhaust pipe 5c, and only the sample gas enters the ion source chamber 8 from the separator outlet 5b and undergoes mass spectrometry.

In the conventional apparatus described above, when replacing the column 1 in a vacuum state, dust in the air is drawn into the separator 5 and blocks the 0.1 mm diameter hole. The exhaust pump and ion source 7 connected to column 5 are cut to expose the column to the atmosphere, and the connecting member 4 is removed to replace the column 1. However, when the device is exposed to the atmosphere, the temperature of the ion source 7 changes, and it usually takes 30 minutes to 1 hour to return to its original stability, and it takes even longer if the temperature conditions are strict. There was a problem.

[Purpose of the invention]

This invention is intended to solve the above-mentioned problems, and includes a gas supply pipe that supplies a replacement gas to the inlet of the separator when replacing a column, and connects it to a connecting member, and also prevents the tailing phenomenon during analysis. It is an object of the present invention to provide a column connection device for a gas chromatography device that can perform column exchange in a vacuum state without inhaling dust by providing a device for introducing a carrier gas into the gas supply pipe.

[Structure of the invention]

This invention relates to a connecting member that connects a column outlet and a separator inlet of a gas chromatography apparatus, a gas supply pipe that connects to the connecting member so as to supply replacement gas to the separator inlet when replacing the column, and A column connection device for a gas chromatography device, characterized in that it includes a device for introducing a carrier gas into the gas supply pipe so as to prevent a tailing phenomenon in the gas chromatography device.

[Embodiments of the invention]

Hereinafter, the present invention will be explained with reference to embodiments of the drawings.

3 and 4 are partial sectional views showing another embodiment of the present invention, and the same reference numerals as in FIGS. 1 and 2 indicate the same or corresponding parts. The connecting member 4 has a structure in which the column outlet part 1b and the separator inlet part 5a are connected to both ends of the connecting pipe 4a, gaskets 4b and 4c are sandwiched between both ends, and the nuts 4d and 4e are tightened. A gas supply pipe 9 is connected to the center of the connecting pipe 4a so that replacement gas can be supplied to the separator inlet 5a during column replacement.

10 is a two-way switching valve, the other end of the gas supply pipe 9 is connected to the common terminal 10a, and the exchange mode terminal 10b is connected to the other end of the gas supply pipe 9.
A replacement gas supply source 13 such as an air cylinder or a compressor is connected to via a filter 11 and a constant pressure valve 12. The above configuration is common to Figures 3 and 4, but
The analysis mode terminal 10c of the switching valve 10 is connected to the exhaust pipe 5c in FIG. 3, and to the carrier gas supply source 15' in FIG. ing.

In the above configuration, the handle 10d of the switching valve 10
When the flow path is switched to the exchange mode terminal 10b by turning , exchange gas such as air is supplied from the exchange gas supply source 13 through the constant pressure valve 12, and after being removed by the filter 11,
The gas enters the connecting pipe 4a of the connecting member 4 through the gas supply pipe 9 from the switching valve 10 and is supplied to the separator inlet portion 5a.

In this state, while continuing to draw vacuum from the exhaust pipe 5c,
The column 1 is replaced by removing the nut 4d of the connecting member 4, and the column replacement is completed by tightening the nut 4d. During this time, the supply of replacement gas from the gas supply pipe 9 continues, so that the dust-removed gas is sucked from the separator inlet 5a, thereby preventing dust-containing air and the like from being sucked in. Further, since the exhaust pipe 5c continues to be evacuated, the ion source 7 maintains a vacuum state.

If analysis is performed in the same state after replacing the column 1, tailing of the solvent and sample will occur due to the dead capacity of the gas supply pipe 9. Therefore, the flow path of the switching valve 10 is switched to the analysis mode terminal 10c and the gas supply pipe A carrier gas for analysis is introduced into the chamber 9 and replaced with an exchange gas. In this case, in FIG. 3, the analysis mode terminal 10c is connected to the exhaust pipe 5C.
Since the exchange gas in the gas supply pipe 9 is discharged to the exhaust pipe 5c at a constant flow rate, a carrier gas for analysis is introduced into the gas supply pipe 9.

The opening degree of the flow rate restriction device 14 is determined by the degree of opening of the flow rate restriction device 14.
40 mΩ/min). In this way, the gas in the gas supply pipe 9 is discharged and replaced with carrier gas, so that no tailing phenomenon occurs. In FIG. 4, several mQ of carrier gas (!(e)) is introduced into the gas supply pipe 9 from another carrier gas supply source 15 through the flow rate restriction device 14 for substitution. After the carrier gas is replaced by the gas, the introduction of the carrier gas into the gas supply pipe 9 may be stopped, but the introduction may be continued during the analysis period.

In the above embodiments, the switching valve 10 of FIG.
The filter 11, constant pressure valve 12, and gas supply source 13 may be omitted, and the flow rate of the flow restriction device 14 may be changed to allow a large amount of carrier gas to flow during column replacement. Further, the structures of the connecting member 4 and the switching valve 10 can also be changed as desired.

〔Effect of the invention〕

According to the present invention, a gas supply pipe for supplying replacement gas to the inlet of the separator when replacing a column is connected to a connecting member, and a carrier gas is introduced into the gas supply pipe to prevent tailing phenomenon during analysis. Since the equipment was installed, columns can be exchanged without inhaling dust in a vacuum state without exposing the ion source to the atmosphere.This allows the temperature conditions inside the ion source to be maintained as is, and also reduces the time required for evacuation and evacuation. This eliminates the need for vacuum cleaners, and provides advantages such as reducing the amount of time it takes to create a high vacuum.

[Brief explanation of drawings]

FIG. 1 is a sectional view of a conventional gas chromatography mass spectrometer, FIG. 2 is a sectional view of its separator, and FIGS. 3 and 4 are partial sectional views showing another embodiment of the present invention. . In each figure, the same reference numerals indicate the same or corresponding parts, 1 is a backed column, 2 is a gas chromatography oven, and 4 is a back column.
1 is a connecting member, 5 is a separator, 6 is a carrier gas introduction pipe, 7 is an ion source, 8 is an ion source chamber, 9 is a gas supply pipe, 10 is a switching valve, 11 is a filter, 13 is a replacement gas supply source, 15 is the carrier gas source. Agent: Patent Attorney Sei Yanagihara (Figure 1, Figure 2)

Claims (4)

[Claims] (1) a connecting member that connects a column outlet and a separator inlet of a gas chromatography apparatus; and a gas supply pipe that connects to the connecting member so as to supply replacement gas to the separator inlet when exchanging force. A column connection device for a gas chromatography device, comprising a device for introducing a carrier gas into the gas supply pipe so as to prevent a tailing phenomenon during analysis. (2) A column connection device for a gas chromatography apparatus according to claim 1, wherein the gas supply pipe is connected to a gas supply source via a filter. (3) A column connection device for a gas chromatography apparatus according to claim 1 or 2, wherein the device for introducing carrier gas discharges a part of the carrier gas for analysis through a gas supply pipe. . (4) A column connection device for a gas chromatography apparatus according to claim 1 or 2, wherein the device for introducing the carrier gas supplies the carrier gas to the gas supply pipe from another carrier gas supply source. .