JPS628526Y2 - - Google Patents

Description

[Detailed Description of the Invention] This invention relates to a sample introduction device for a liquid chromatograph, and more particularly to an apparatus for concentrating a low concentration sample and introducing it into a column of a liquid chromatograph.

Conventionally, when subjecting a low-concentration sample to liquid chromatography, the sample's dilution solvent is evaporated and concentrated in advance, and the concentrated liquid is then injected into the sample injection section of the liquid chromatograph, or the low-concentration sample is A large amount of the sample was injected into the sample injection section of a liquid chromatograph.

However, the former method has the drawback of being time consuming and complicated to operate, while the latter method has the drawback of having a limit on the amount of injection and cannot be applied to samples with fairly low concentrations.

This invention was made in view of the above circumstances, and provides a sample introduction device with a novel configuration that does not have the above-mentioned drawbacks.

This invention will be explained in detail below based on the embodiment shown in the drawings.

1 shown in FIG. 1 is an embodiment of the liquid chromatograph sample introduction device of this invention.

A carrier liquid supply section 4 is constituted by the carrier liquid tank 2 and the liquid sending pump 3.
is connected to one port a of the hexagonal connector 8.

5 is an inert gas cylinder, which is connected to one port c of the hexagonal tank 8 via a valve 6.
These inert gas cylinder 5 and valve 6 constitute an inert gas supply section 7.

The hexagonal cock 8 has ports b, d, e, f in addition to the ports a, c, and in its first position (the flow path position indicated by the broken line in Figure 1), the ports a, b, c
and d, e and f are electrically connected, and in the second position (the flow path position indicated by the solid line in Figure 1), ports a and f, b and c, and d and e
conducts.

The carrier inlet 10 of the sample injection tube 9 is connected to the port b of the hexagonal socket 8, and the sample outlet 1
1 is connected to port e. A heater 13 is also provided along the sample injection tube 8.

The column 14 of the liquid chromatograph is connected to the port f of the hexagonal tank 8, and the exhaust part 15 is further connected to the port d of the hexagonal tank 8. The exhaust section 15 is, for example, an exhaust path open to the atmosphere.

When using this device 1, first close the valve 6 of the inert gas supply section 7, set the hexagonal pot 8 to the second position (solid line), insert the syringe M into the septum 12, and inject a diluted sample with a low concentration. Inject into the sample injection tube 9. Next, the valve 6 is opened to allow inert gas to flow into the sample injection tube 9, and the diluted sample is heated by the heater 13. Then, the diluent solvent is vaporized, transported with an inert gas, and exhausted from the exhaust section 15. There, the sample is placed in the sample injection tube 9.
It will be concentrated inside. When the diluent solvent is sufficiently exhausted, close the valve 6, fill the sample injection tube 9 with carrier liquid using another syringe, and switch the hexagonal pot 8 to the first position (dashed line). If a carrier liquid is supplied from the carrier liquid supply section 4, the sample in the sample injection tube 9 is introduced into the column 14 of the liquid chromatograph in a concentrated state.

If the target component and interfering component coexist in the sample, close the valve 6 after the dilution solvent is sufficiently exhausted, and use another syringe to add a solvent that dissolves only the interfering component without dissolving the target component. Sample injection tube 9
Inject inside. Then, the interfering components are dissolved and exhausted from the exhaust section 15. Then, use another syringe to add carrier fluid to the sample injection tube 9.
Fill the inside and place the hexagonal pot 8 in the first position (dashed line)
When the carrier liquid is supplied from the carrier liquid supply section 4, the target component is introduced into the column 14 of the liquid chromatograph in a concentrated state.

FIG. 2A shows an example of the results of concentrating a diluted sample with a low concentration as described above and analyzing it using a high performance liquid chromatograph. The diluted sample was prepared by diluting diphenyl with methanol. In contrast, Figure 2B shows the results of analyzing the same diluted sample as above using the conventional method of evaporating the diluting solvent of the sample in advance to concentrate it and then injecting it into a high-performance liquid chromatograph for analysis. be.
Comparing these, it can be seen that the device of this invention can quickly obtain the same analytical results as the conventional method with a simpler operation than the conventional method.

As understood from the above description, the liquid chromatograph sample introduction device of this invention connects the carrier liquid supply section and the inert gas supply section to the carrier inlet of the sample injection tube via the carrier switching means, and The present invention is characterized in that the sample injection port of the sample injection tube is connected to the column and exhaust section of the liquid chromatograph via a destination switching means, and the sample injection tube is provided with a heating means.

Therefore, by heating the diluted sample injected into the sample injection tube with a heating means, and supplying an inert gas into the sample injection tube and exhausting it from the exhaust part,
Samples can be easily concentrated. Furthermore, by switching the carrier switching means and the destination switching means, the concentrated sample can be quickly introduced into the column of the liquid chromatograph.

Ultimately, these methods make it possible to analyze low-concentration samples by liquid chromatography more easily and quickly than in the past.

Note that when the sample does not require concentration, it is only necessary to supply no inert gas from the inert gas supply section, and the analysis can be performed in the same manner as described above.

Another example is one in which a pressure reducing device such as a vacuum pump or an aspirator is added to the exhaust section to reduce the pressure inside the sample injection tube. This is preferable because it promotes vaporization of the diluent solvent.

[Brief explanation of the drawing]

Figure 1 is an explanatory diagram of the configuration of one embodiment of the liquid chromatograph sample introduction device of this invention, Figure 2A is a chromatogram of an example of analysis performed using the device of this invention, and Figure 2B is a conventional example. This is a chromatogram of an example of analysis carried out by the method. 1...Sample introduction device for liquid chromatograph, 4
... Carrier liquid supply section, 7 ... Inert gas supply section, 8 ... Roxagonal pot, 9 ... Sample injection tube, 10
...Carrier inlet, 11...Sample sending port, 13...
...Heater, 14...Liquid chromatograph column, 15...Exhaust section.

Claims (1)

[Claims for Utility Model Registration] 1. Connecting the carrier liquid supply section and the inert gas supply section to the carrier inlet of the sample injection tube via a carrier switching means, and connecting the sample outlet of the sample injection tube to the column of a liquid chromatograph. and a sample introduction device for a liquid chromatograph, characterized in that the sample introduction device is connected to the exhaust section via a destination switching means, and the sample injection tube is provided with a heating means. 2 Carrier switching means and destination switching means are 1
The hexagonal socket has ports a to f, and in the first position ports a and b, ports c and d, and ports e and f are electrically connected, and in the second position Ports a and f, ports b and c, and ports d and e are electrically connected,
The carrier liquid supply section is connected to port a, the inert gas supply section is connected to port c, the carrier inlet of the sample injection tube is connected to port b, the sample delivery port of the sample injection tube is connected to port e, and the liquid chromatograph column is connected to port f. 2. The device according to claim 1, wherein the exhaust section is connected to port d.