JPH01165953A - Liquid chromatograph - Google Patents

Abstract

PURPOSE:To enable the collection of a refined component without a loss of a sample, by providing a check valve to prevent the backflow of a liquid to a solvent reservoir and also by providing a capacity variable chamber in a channel connecting a detector and a pump together. CONSTITUTION:An eluant is supplied from a solvent reservoir 1 to a column 4 by a pump 2. A sample is injected from a sample injection device 3, separated by the column 4 and detected by a detector 5. Next, an eluate from the detector 5 is led to a recycle valve 6. A separated component is collected or it is circulated again through the pump 2 to be subjected to re-chromatography in the case when the separation is insufficient. The collection of the sample or the execution of the re-chromatography is effectuated herein by a switching operation of the valve 6. When the recycle chromatography is implemented, an eluate from the valve 6 passes through a capacity variable chamber 9 and is sucked by the pump 2. When the pump 2 is in a suction stop process, the eluate is reserved in the variable chamber 9. In this case, the flow of the eluate toward the reservoir 1 is prevented by a check valve 8.

Description

DETAILED DESCRIPTION OF THE INVENTION [Field of Industrial Application] The present invention relates to a liquid chromatograph, and particularly to a liquid chromatograph suitable for carrying out recycling chromatography.

[Conventional technology]

As described in the document "Handbook of High-Performance Liquid Chromatography" edited by Takebe Yamabe (Saiwai Shobo), when performing recycling chromatography, conventional equipment connects the flow path connecting the detector and pump, and the solvent reservoir and pump. There was continuity with the connecting channel.

[Problem that the invention seeks to solve]

The above-mentioned conventional technology does not take into consideration the fact that the sample components are diffused toward the solvent reservoir during the process in which the sample components are guided from the detector to the pump, resulting in the problem of contamination of the sample components. That is, the liquid pumped from the detector through the recycle valve is a continuous flow, whereas the pump does not draw in liquid continuously. In other words, since suction is only performed intermittently, the eluate from the detector flows back toward the solvent reservoir while the pump is not suctioning. When the pump enters the suction process, this backflow is either sucked into the pump, or as the backflow and suction are repeated, part of the eluate diffuses toward the solvent reservoir, and the recycling operation ends. When moving on to the operation of collecting the structural components in the test tube, the eluent is supplied from the solvent reservoir, or the sample components that have diffused and remained in the flow path are sucked into the pump and the column is removed. Since it is detected by a chromatogram, it appears as a peak on the chromatogram. There is a danger that regular customers of this ghost peak may mistake it for an unknown component peak, and fatal problems such as overlapping with the target component peak may occur, causing contamination.

An object of the present invention is to prevent sample components, ie, eluate, from flowing back and diffusing toward the solvent reservoir when recycling chromatography is performed.

[Means for solving problems]

The above object is achieved by providing a check valve that prevents liquid from flowing back into the solvent reservoir, and by providing a means for varying the volume of the flow path in the flow path connecting the detector and the pump.

[Effect]

The check valve prevents the eluate from flowing from the detector toward the pump, and prevents it from flowing back toward the solvent reservoir. Further, the variable volume means operates to accumulate liquid continuously eluted from the detector when the pump is in the suction stop process. As a result, the liquid eluted from the detector passes only through the pipe connected to the pump and is sucked into the pump, so that ghost peaks and contamination do not occur.

〔Example〕

An embodiment of the present invention will be described below with reference to FIGS. 1 and 2. FIG. 1 is an embodiment showing the entire apparatus of the present invention. Pump 2 pumps the eluent from Turben 1 to Reservoir 1 to Column 4.
Send liquid to. A sample is injected from a sample injection device 3, separated by a column 4, and detected by a detector 5. The eluate discharged from the detector 5 is guided to a recycle valve 6, and the separated components are collected in a test tube 7, or if the separation is insufficient, the eluate is circulated through the pump 2 again to perform re-chromatography. Whether to collect the sample or perform re-chromatography is determined by switching the recycle valve 6. When performing recycle chromatography, the eluate discharged from the recycle valve 6 passes through the variable volume chamber 9, reaches the pump 2, and is sucked. When the pump 2 is in the suction stop stroke, the eluate accumulates in the variable volume chamber 9. In this case, the check valve 8 prevents the eluate from flowing toward the solvent reservoir 1 . When the pump 2 moves to the suction stroke, the eluate accumulated in the variable volume chamber is sucked into the pump 2, and at the same time, its volume is reduced. FIG. 2 shows an embodiment of the check valve 8 and the variable volume chamber 9.

The check valve consists of a valve seat 10 and a ball 11. When the liquid flows toward the solvent reservoir 1, the ball 11 closes to the valve seat 1o.
Seal and cut off the flow. The variable volume chamber 9 consists of a liquid chamber 12 and an elastic body 13, and the elastic body 13 reduces its volume by the pressure of the liquid. The elastic body 13 may have, for example, a hollow elastic body filled with compressed air.

According to this embodiment, when the eluate discharged from the detector 5 is recycled, all peak components are returned to the column 4 via the pump 2 again, since the liquid does not diffuse into the branch path. In other words, a completely closed flow path system is formed and the liquid circulates only within this closed flow path system, which has the effect of preventing contamination and the appearance of ghost peaks.

〔Effect of the invention〕

According to the present invention, all of the eluate from the detector is sucked into the pump without diffusing into the solvent reservoir, which prevents contamination and the appearance of ghost peaks, and replenishes purified components without sample loss. It has the effect of being able to collect

[Brief explanation of the drawing]

FIG. 1 is an explanatory diagram showing the entire apparatus according to an embodiment of the present invention, and FIG. 2 is an explanatory diagram showing the part of the present invention in FIG. 1...Solvent reservoir, 2...Pump, 3...
Sample injection device, 4... Column, 5... Detector, 6...
・Recycle valve, 7...Test tube, 8...Check valve, 9...Volume 1st hole 2 Figure 11, 6 Solvent soap °-8 = g, , Recycle valve 2...・Talented skills 7.
1. Six people, Tobuki Kanri 43. Sample loading device &...
Shojo sho 4 --- Power 919. Togai, 7 Nemachi Hen (59, Fusen Tain)

Claims (1)

[Claims] 1. In a liquid chromatograph consisting of a solvent reservoir, a pump, a sample injection device, a column, and a detector, a flow path switching valve is provided to select whether to collect the eluate from the detector or guide it to the pump, and the detection 1. A liquid chromatograph, comprising means for varying the volume of a flow path between a solvent reservoir and a pump, and a check valve provided in a flow path between a solvent reservoir and a pump.