JPH06167481A - Process liquid chromatograph - Google Patents

Abstract

PURPOSE:To prevent a malfunction of a pumping operation by suppressing generation of bubbles from eluate. CONSTITUTION:An eluate tank 28 is formed in an upper part in a soaking block 40 of a constant temperature bath, a feed pump 30 is disposed in a lower part, and an eluate outlet at a bottom of the tank 28 is connected to the pump 30 via a pipe 38. An outside of the block 40 is covered with a heat insulator 50. Steam of a predetermined temperature is supplied from an exterior to the block 40 through a flow regulating valve 52, which is regulated by a temperature controller 54, and the bath is maintained at a predetermined temperature.

Description

Detailed Description of the Invention

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a process liquid chromatograph which is connected to a process line of the chemical industry and which can sample and analyze samples online from the process side.

[0002]

2. Description of the Related Art A liquid chromatograph is equipped with a separation column, an injector for collecting a sample and sending it to the separation column, and a detector for detecting the components eluted from the separation column. The sample collected by the injector is sent to the separation column for separation. In order to separate each component in the column, a separation analysis is performed while the eluent is flowed as a mobile phase.

The eluent is contained in the eluent tank, and the eluent tank and the liquid feed pump are connected by a liquid feed pipe.
The eluent is sucked by a liquid feed pump and supplied to the separation column through an injector or directly. The eluent tank, the liquid feed pipe, and the liquid feed pump are connected to each other, but are used in the state of being exposed to the outside air. In particular, since the process liquid chromatograph is often installed outdoors, the eluent tank, the liquid feeding pipe, and the liquid feeding pump are directly affected by the temperature change due to the fluctuation of the outside air temperature.

[0004]

Nitrogen, oxygen, carbon dioxide, etc. in the air are dissolved in the eluent. In process liquid chromatographs that are often directly connected to outdoor plants, the dissolved gas in the eluent becomes bubbles due to rapid changes in the outside temperature, and these bubbles enter the liquid delivery pump such as a plunger pump and stop the pumping action. Sometimes. It is an object of the present invention to suppress the generation of bubbles from the eluent in a process liquid chromatograph and prevent the pump action from becoming defective.

[0005]

In the present invention, at least the eluent tank, the liquid feed pump, and the liquid feed pipes between the eluent tank and the liquid feed pump are integrated and housed in a constant temperature bath.

[0006]

[Function] By integrating the eluent tank, the liquid feed pump, and the pipes connecting them, and keeping them at the same temperature by the constant temperature tank, the eluent tank, the pump and the pipe can be maintained even if the ambient temperature fluctuates. There is no temperature distribution between the classes, and therefore the generation of bubbles in the eluent due to changes in the outside temperature is suppressed.

[0007]

EXAMPLE FIG. 1 shows a process liquid chromatograph of one example. Reference numeral 2 is a reactor of a process line, and the process line 2 is connected to a circulation channel including a pump 4 and a cross-flow type ceramic filter 6. A diluting valve 10, which is a six-way valve, is connected to the filtrate outlet of the filter 6 via a sample pump 8. The diluting valve 10 is provided with a metering loop 12, a mixer 14 for diluting a sample is connected to the diluting valve 10, a diluting liquid pump 18 for supplying a diluting liquid 16 is connected, and a drain passage to a drain 19 is also connected. ing. The outlet of the mixer 14 is connected to an injector 20 of a high performance liquid chromatograph (HPLC). The injector 20 is of a six-way switching valve type and has a metering loop 22. The sample supplied from the mixer 14 to the injector 20 and not injected into the column 24 is discharged to the drain 26. Injector 20
The column is connected with a liquid feed pump 30 for supplying the eluent stored in the eluent tank 28 to the HPLC. Three
2 is a detector and 34 is a data processing device.

The eluent bath 28, the liquid feed pump 30, and the pipe connecting them are integrated and housed in a constant temperature bath 36. In order to collect the sample diluted by the mixer 14 of the diluting device with the injector 20 and introduce it into the column 24, the injector 20 causes the sample to flow from the metering loop 22 to the drain 26 according to the flow path of the solid line, and the sample is mixed with the metering loop 22. Injector 2
0 is switched to the flow path indicated by the broken line, and the sample is sent to the column 24 by the eluent 28.

FIG. 2 shows an example in which the eluent tank 28, the liquid feed pump 30, and the pipe 38 therebetween are integrated and housed in a constant temperature tank in the embodiment. The eluent bath 28 is formed in the upper part of the soaking block 40 of the constant temperature bath, and the liquid feed pump 30 having two pump heads 30a and 30b is arranged in the lower part. An eluent outlet is provided at the bottom of the eluent tank 28, and a pipe 38 is connected between the eluent outlet and the inlets of the pump heads 30a and 30b. At the bottom of the constant temperature bath, both pump heads 30
The pipes 42 connected to the outlets of a and 30b join and are guided to the outside, and pass through the injector 20 of FIG.
It is led to 4. An eluent supply port 44 is provided at the upper end of the eluent tank 28, and an eluent 48 is supplied via an opening / closing valve 46.

The outside of the soaking block 40 is covered with a heat insulating material 50. Steam having a constant temperature is supplied to the soaking block 40 from the outside via a flow rate adjusting valve 52, and a temperature controller 54 is provided to adjust the flow rate adjusting valve 52. A temperature sensor 56 is arranged in the eluent tank 28, and the detection output of the temperature sensor 56 is the temperature controller 5.
4, the flow rate adjusting valve 52 is adjusted so that the temperature detected by the temperature sensor 56 becomes constant, and the steam supply to the soaking block 40 is controlled. By controlling the flow rate of steam, the temperature of the soaking block 40 is kept constant, and the temperature of the eluent 48 inside the soaking block 40 and the temperature of the pump 30 and the pipe 38 are kept constant regardless of changes in the external temperature. The structure in which the eluent tank, the liquid feed pump, and the pipes between them are integrated and housed in the constant temperature tank is not limited to that shown in FIG. 2, and can be variously modified.

[0011]

According to the present invention, since the eluent tank, the pump for feeding the eluent and the pipe between them are integrally housed in the constant temperature tank, no temperature difference occurs between them. As a result, it is possible to prevent the dissolved gas of the eluent from forming bubbles and hindering the pumping action even when the outside air temperature changes. Process liquid chromatographs are often used outdoors,
Therefore, the outside air temperature may drop below the freezing point of the eluent, but by the present invention, the eluent is frozen by storing the eluent tank, the liquid feed pump and the pump between them in a constant temperature tank and keeping them at a constant temperature. It is also possible to prevent the liquid chromatograph from becoming inoperable.

[Brief description of drawings]

FIG. 1 is a channel diagram showing a process liquid chromatograph of one example.

FIG. 2 is a cross-sectional view showing an eluent tank, a pump, and a pipe between them, which are housed in a constant temperature tank in the embodiment.

[Explanation of symbols]

 2 Reactor of process line 10 Dilution valve 20 Injector 24 Separation column 28 Eluent tank 32 Liquid feed pump 32 Detector 36 Constant temperature bath 40 Constant temperature soaking block 50 Constant temperature insulation material

Claims (1)

[Claims] 1. A liquid chromatograph having a separation column, an injector for collecting a sample and sending it to the separation column, and a detector for detecting an elution component from the separation column, and a liquid chromatograph for collecting and diluting a sample from the process side. In a process liquid chromatograph equipped with a sample introducing section for introducing into a graph, an eluent tank for an eluent supplied to a separation column via the injector, a liquid feed pump for supplying the eluent to the injector, and the eluent tank. A process liquid chromatograph, characterized in that a portion including at least a liquid feeding pipe between the liquid feeding pump and the liquid feeding pump is integrated and housed in a thermostatic chamber.