JPH09145701A - Liquid chromatograph - Google Patents

Abstract

(57) [PROBLEMS] To provide a liquid chromatograph device having a simple structure and capable of promptly detecting a leak in a flow path of the entire system and provided with safety measures. SOLUTION: A flow rate setting means 20 for setting a flow rate of a liquid delivered by a liquid delivery pump 10, a control means 23 for controlling the liquid delivery pump so that the flow rate set by the flow rate setting means 20 is delivered, and a most downstream side. Flow sensor 16 provided at a position downstream of the component in
Is provided with a comparison unit 22 that compares the flow rate value measured by the flow rate setting unit 20 with the set flow rate set by the flow rate setting unit 20. According to the result of the comparison unit 22, there is liquid leakage when the measured flow rate value is smaller than the set flow rate value. To judge.

Description

Detailed Description of the Invention

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a liquid chromatograph device, and more particularly to a liquid chromatograph device having a liquid leakage monitoring function.

[0002]

2. Description of the Related Art A liquid chromatograph apparatus generally includes a liquid feed pump, an injector, a column, a column oven,
The system is configured by connecting each component such as a detector. In some liquid chromatograph devices, each component is prepared as an independent component, and there is a liquid chromatograph device system in which necessary components are combined. For example, for the liquid delivery pump, select the appropriate component from the liquid delivery pump components that have multiple types such as single plunger pump or double plunger pump, large flow pump or small flow pump, and Is selected from among a manual injector or an auto-injector, and a detector is selected from an ultraviolet visible light detector, a fluorescence detector, a chemiluminescence detector, a differential refractometer detector, a conductivity detector, etc. Mobile phase box (with mobile phase tank installed inside), liquid transfer pump, injector,
The system is configured by connecting each of the components of the column oven (internally mounting the column), the detector, and the control unit, and the gradient unit is added to this to configure the gradient system. Or
A system suitable for measurement can be configured by adding a fraction collector.

By the way, in the liquid chromatograph apparatus,
Although a solvent is used as the mobile phase, flammable solvents are often used, and safety measures against liquid leakage are necessary. Particularly in recent years, unmanned continuous operation has become more frequent, and the importance of consideration for safety is increasing.

Conventionally, as a safety measure against liquid leakage,
Each component such as the liquid feed pump, detector, column oven, etc. is equipped with a leak sensor to detect liquid leaks.When a liquid leak occurs inside each component, each leak sensor detects it. A safety system was used to take measures such as stopping the pump.

[0005]

In the conventional safety system, a safety measure was taken to detect a liquid leak by providing a leak sensor for each component. Therefore, it is possible to detect a liquid leak inside each component, but it is not possible to detect when there is a liquid leak in the piping between the components, and no matter where in the entire system the liquid leak occurs, The system was not able to detect leaks.

Further, even if there is a liquid leak inside the component, due to the position where the leak sensor is installed and the sensitivity of the leak sensor itself, a considerable amount of time is required from when the leak actually occurs until when the leak sensor detects it. In some cases, there was a delay in response.

Further, if a leak sensor is provided for each component, a plurality of leak sensors are required, which is wasteful and the wiring becomes complicated, which not only causes erroneous wiring, but also the device. It has also become a factor of high cost.

The present invention solves the above problems, and even if a liquid leak occurs anywhere in the entire system of a liquid chromatograph apparatus configured by combining each component, the liquid leakage can be prevented by a simple safety system. An object of the present invention is to provide a liquid chromatograph device capable of rapid detection.

[0009]

The liquid chromatograph apparatus of the present invention, which has been made to solve the above problems, is constituted by connecting a plurality of separated components including at least a liquid feed pump section through a flow path. In the liquid chromatograph device, flow rate setting means for setting the flow rate of the liquid sent out by the liquid sending pump section, control means for controlling the liquid sending pump so that the flow rate set by the flow rate setting means is sent, and the most downstream side A flow rate sensor provided at a position downstream of a component, a flow rate value measured by the flow rate sensor, and a comparison means for comparing the set flow rate set by the flow rate setting means are provided. It is characterized in that the presence or absence of liquid leakage of the chromatographic device is determined.

In the liquid chromatograph device of the present invention, the liquid feed pump is controlled by the control means so that the liquid feed pump on the upstream side of the liquid feed passage has the flow rate set by the setting means. On the other hand, a flow rate sensor is provided at the most downstream side of the liquid sending flow path, and the flow rate of the liquid being sent is measured by this. Then, the set flow rate and the measured value of this flow rate sensor are compared by the comparison means.

When there is no liquid leakage, the set flow rate, which is the flow rate delivered from the liquid delivery pump, and the flow rate measured by the flow rate sensor located at the most downstream side of the flow path match, and therefore have the same value. If liquid leakage occurs in the flow path, the flow rate value measured by the flow rate sensor will be less than the set flow rate. Therefore, the presence or absence of liquid leakage can be determined by comparing the set flow rate and the flow rate value measured by the flow rate sensor by the comparison means.

Moreover, the position of the liquid leak is not limited to the inside of the component, and the liquid leak can be detected wherever the liquid leak occurs at a place of the flow path downstream of the liquid feed pump and upstream of the flow rate sensor. .

[0013]

DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS An embodiment of the present invention will be described below with reference to the drawings. FIG. 1 is a configuration diagram showing a liquid chromatograph device showing an embodiment of the present invention.

In the figure, 10 is a liquid feed pump, 11 is an injector for injecting a sample, 12 is a column, 13
Is a column oven for adjusting the temperature of the column 12, and 14 is a detector. Each of these is independently configured as a component. And made of SUS or PEEK
By connecting the flow path in the middle from the mobile phase tank to the drain by a pipe made by, and further by mounting the flow rate sensor 16 on the flow path further downstream than the detector 14 which is the most downstream component, The entire channel of the liquid chromatograph device of the embodiment is formed. Fifteen
Is a power supply device for operating each component of the liquid feed pump 10, the injector 11, the column oven 13, and the detector 14.

Reference numeral 17 denotes a computer system for controlling the present liquid chromatograph apparatus, which is a keyboard for inputting setting parameters such as a flow rate, a CR for displaying a control state and outputting an alarm display.
It has ordinary computer hardware such as T, a CPU for performing various calculations and control calculations, and a memory. Explaining the function of the computer 17, the keyboard functions as the flow rate setting means 20, and the CR
T functions as the display unit 21, and the CPU and the memory function as the comparison unit 22 and the control unit 23.

Next, the operation of the present invention will be described with reference to the flowchart of FIG. First, when the set flow rate of the liquid feed pump 10 is input from the keyboard (ST1), the computer 17 executes liquid feed control so that the flow rate delivered from the liquid feed pump 10 becomes the set flow rate (ST2).
At this time, the flow rate sensor 16 on the downstream side of the flow path continues to monitor the actual flow rate of the liquid (ST3). And
The measured flow rate of the flow rate sensor 16 is compared with the set flow rate (ST
4) When these are almost the same, it is judged that there is no liquid leak, and the liquid feed is continued while monitoring the liquid leak. On the other hand, when the measured flow rate of the flow rate sensor 16 is clearly smaller than the set flow rate, it is determined that there is a liquid leak, and then necessary safety measures are executed. In the present embodiment, the liquid supply is automatically stopped by sending a power supply stop signal from the computer 17 to the power supply device 15 (ST5). At the same time, by displaying that the liquid leak has occurred on the CRT, the measurer is notified that the liquid leak has occurred. By doing this, disasters can be prevented.

In this embodiment, when liquid leakage is detected,
Liquid feed pump 10, injector 11, column oven 1
3. Each component constituting the liquid flow path system of the detector 14 is stopped, but not limited to this, only the liquid feed pump may be stopped, or conversely the entire system may be stopped. .

[0018]

As described above, in the liquid chromatograph apparatus of the present invention, it is possible to detect liquid leakage at any place in all the flow paths of the system, and no liquid leakage sensor is used. Therefore, there is no problem such as delay in response due to sensitivity characteristics or sensor position, and liquid leakage can be found quickly. Further, since it is sufficient to use only one flow rate sensor, the safety measure system can have an extremely simple structure. Furthermore, even if the combination of the components that make up the liquid chromatograph device is changed, no matter what the combination is, it is only necessary to install the flow rate sensor at the most downstream position. it can.

[Brief description of the drawings]

FIG. 1 is a configuration diagram of a liquid chromatograph apparatus according to one embodiment of the present invention.

FIG. 2 is a flowchart of the liquid chromatograph device of the present invention.

[Explanation of symbols]

 10: Liquid sending pump 11: Injector 13: Column oven 14: Detector 15: Power supply device 16: Flow rate sensor 17: Computer 20: Flow rate setting means 21: Display means 22: Comparison means 23: Control means

Claims (1)

[Claims] 1. A liquid chromatograph apparatus constituted by connecting a plurality of separated components including at least a liquid feed pump section in a flow path, and a flow rate setting means for setting a flow rate of a liquid delivered by the liquid feed pump section. , A control unit for controlling the liquid feed pump so that the flow rate set by the flow rate setting means is sent, a flow rate sensor provided at a position on the downstream side of the most downstream component, and a flow rate value measured by the flow rate sensor. And a comparison means for comparing the set flow rate set by the flow rate setting means, and the presence or absence of liquid leakage of the liquid chromatograph apparatus is determined based on the result of the comparison means. apparatus.