JP3324299B2 - Liquid chromatograph - Google Patents

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to an integrated liquid chromatograph.

[0002]

2. Description of the Related Art As shown in FIG. 5, a conventional liquid chromatograph 50 has a pump unit 51 containing a liquid feed pump 60 and an injector 61, a column 62 and a detector 63.
And a control unit 53 that houses a circuit for controlling them, and a constant temperature unit 52 that holds them at a constant temperature.

[0003]

As described above, when each unit is independent, tubes and pipes for transferring liquid between the units, electric wiring for transmitting electric power and signals, and the like are correctly provided. They had to be connected and the installation of the device was very cumbersome. In a liquid chromatograph, it is desirable that the distance between the injector for injecting the sample and the column be as short as possible.However, in a conventional apparatus, since these are included in a separate unit, the sample is easily diffused between them and high precision There was also a problem that analysis was difficult.

Further, the control unit 53 is provided with a circuit capable of performing simple data processing. However, when performing complicated data processing such as identifying a component name corresponding to each peak, the control unit 53 is separately provided. An advanced data processing device 55 such as a personal computer had to be connected, and a large floor space was required to install the entire device.

The present invention has been made in order to solve such a problem, and an object of the present invention is to perform a highly accurate analysis while being compact and easy to handle. It is an object of the present invention to provide a liquid chromatograph device which can be used.

[0006]

The liquid chromatograph apparatus according to the present invention, which has been made to solve the above problems, comprises: a) a liquid sending pump for sending a mobile phase to a column; b) a column and a detector. A) a constant temperature unit disposed therein; c) a control circuit for controlling the liquid feed pump, the constant temperature unit and the detector, and performing predetermined data processing based on a detection signal generated by the detector; and It has a space for accommodating the liquid sending pump and the constant temperature unit, a space for accommodating the mobile phase container and the waste liquid container, and an inlet for a sample injector is provided on the outer surface, and a door for opening and closing the front opening. A housing provided with an input unit for inputting commands to the control circuit and a display unit for displaying data generated by the control circuit on an outer surface; e) a liquid feed pump, a sample injector, a column, and a detection unit Pipes to connect the It is characterized in that to obtain.

[0007]

[Operation] When performing an analysis, the space in the housing is
A container for storing the mobile phase and a container for storing the waste liquid are put therein. The liquid sending pump sucks the mobile phase in the mobile phase container and sends it to the column via the sample injector. When the operator injects a sample from the inlet of the sample injector provided on the outer surface of the housing, the sample is transferred to the column by the mobile phase. Each component of the sample is separated in a column and detected by a detector. The waste liquid from the detector is discharged to a waste liquid container. During this time, the control circuit controls the operation of the pump, the operation for temperature control in the constant temperature unit, and the operation of the detector, and also performs various data processing by analyzing a detection signal output from the detector. Information indicating data processing results, analysis conditions, and the like are displayed on a display unit provided on an outer surface of a door that opens and closes an opening on a front surface of the housing. Commands to the control circuit are also issued from an input unit provided on the outer surface of a door that opens and closes the opening of the housing.

[0008]

DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS A portable liquid chromatograph according to one embodiment of the present invention will be described with reference to FIGS. As shown in FIG. 1, the housing 11 of the liquid chromatograph device 10 of the present embodiment has a substantially rectangular parallelepiped shape, and one surface thereof (FIG. 1).
(The left side in (a)).
As shown in FIG. 1B, two doors 12 and 13 are provided on the front surface, which is the opening of the housing 11, and one of the doors (hereinafter referred to as a main door) 12 is substantially the opening. The other door (hereinafter, referred to as a sub door) 13 occupies the remaining １ ／. The two doors 12 and 13 open in a double-opening manner around rotating shafts 114 and 116 provided on the left and right sides of the opening, respectively, to open the opening of the housing 11.

The main door 12 is configured to have a certain thickness, and a control circuit 45 for controlling the operation of the entire chromatographic apparatus 10 and performing data processing on the detected chromatogram is provided inside the main door 12. Have been. An LCD panel 121 as a display unit of the control circuit 45 and a keyboard 122 as an input unit are provided on the upper front part of the main door 12, and an external storage device is provided on the side (see FIG. 1C). 3.5 inch floppy disk drive (FDD) 123 is provided.
It should be noted that a touch panel is provided on the surface of the LCD panel 121, and input can also be performed from this touch panel (the LCD panel 121 and the control circuit 45 in FIG. 4).
Between the two arrows). As shown in FIG. 1 (c), the visibility of the LCD panel 121 and the operability of the keyboard 122 are improved by slightly inclining the upper front part of the main door 12. A latch button 115 for unlocking the main door 12 is provided at an upper end of the main door 12 opposite to the rotation shaft 114.

A drain valve 15 with a pressure sensor and an injector (injector) 16 are provided on the front face of the sub door 13, and an opening 131 with a lid for maintaining these valves is provided on the side face. Have been. In the liquid chromatograph apparatus of the present embodiment, the small auxiliary door 13 is provided separately from the main door 12, so that the injector 16 can be provided near the rotation shaft 116 of the auxiliary door 13. Therefore, the moving distance of the injector 16 when the door 13 is opened can be reduced, and the injector 16 and the column 3 can be moved.
5 can be minimized. Thereby, the diffusion of the sample between the injection and the separation of the column can be minimized.

On the upper surface of the housing 11, a mobile phase container 22 described later is provided.
And an opening 1 for accommodating the waste liquid container 23 in the housing 11
11 are provided. 112 is a lid for the opening 111. A handle 113 is provided substantially at the center of the upper surface of the housing 11, so that the liquid chromatograph device 10 of the present embodiment is portable.

As shown in FIG. 2, inside the housing 11,
The liquid feed pump 20 and the constant temperature unit 21 are housed. In this embodiment, a double plunger type pump is used as the liquid sending pump 20, but another type of pump may be used. Behind the constant temperature unit 21, the mobile phase container 2
2 and a space for accommodating the waste liquid container 23 are provided. The opening 111 is provided above this space.

As shown in FIG. 3, the constant-temperature unit 21 forms a substantially rectangular parallelepiped closed space with a box-shaped main body 31 made of a heat insulating material and a door 32 made of a thick heat insulating material. Inside the space, a heater 40 and an aluminum heat equalizing plate 3 for uniformly transmitting the heat generated by the heater into the space are provided.
3 are provided. A column holder 34 that holds a column 35 and a detector 36 that measures the electric conductivity of the liquid that has passed through the column 35 are fixed to the heat equalizing plate 33. In this embodiment, an electric conductivity meter is used as a detector, but another detector may be used. The column 35 is vertically fixed to the column holder 34 by a fixture 41. In the chromatographic apparatus of the present embodiment, the floor area of the entire apparatus is reduced by vertically arranging the vertically long constant temperature unit 21 in which the column 35 is housed vertically. Near the column 35, a temperature sensor 43 for detecting the temperature inside the constant temperature unit 21 is provided. The door 32 of the constant temperature unit 21 can be opened and closed by a hinge 37 and a handle 38.

The above components are connected as shown in FIG. First, a drain valve 15 provided on the sub door 13 is provided between the liquid sending pump 20 and the inlet of the column 35.
And the injector 16 are connected in this order. The constant temperature unit 21 is provided with a liquid inlet and a liquid outlet, and the column inlet is connected to the liquid inlet of the constant temperature unit 21. Therefore, the injector 16 is connected to the liquid inlet of the constant temperature unit 21. Similarly, the outlet of the detector 36 is connected to the liquid outlet of the constant temperature unit 21. The injector 16 is provided with a sample loop 17 for temporarily holding the injected sample, and the injector 16 switches the flow path between a path that passes through the sample loop 17 and a path that does not pass. Is provided. Reference numeral 161 denotes an operation lever of the switching valve.

When analyzing a sample with this apparatus, first,
The mobile phase container 22 and the waste liquid container 23 are stored in the space behind the constant temperature unit 21 through the opening 111 on the upper surface of the housing 11. The suction tube 1 having one end connected to the suction port of the liquid sending pump 20 in the mobile phase liquid in the mobile phase container 22.
9 is input. A filter is provided at the tip of the tube 19. Next, the tip of the tube connected to the liquid outlet of the constant temperature unit 21 (that is, connected to the detector 36) is put into the waste liquid container 23.

After the above preparation, when the operator instructs the start of measurement from the keyboard 122, the control circuit 45 first supplies power to the heater 40 while monitoring a signal from the temperature sensor 43 in the constant temperature unit 21. By doing so, the inside of the constant temperature unit 21 is controlled to a predetermined temperature. When the temperature in the constant temperature unit 21 is stabilized, the operation of the liquid sending pump 20 is started, and the mobile phase is sent to the column 35. At this time, the liquid sending pressure is checked by a pressure sensor provided in the drain valve 15. After the liquid sending is started, the operator injects the sample from the injector 16.
The injected sample is temporarily held in the sample loop 17,
When the operator rotates the lever 161, the sample is pushed out of the sample loop 17 to the column 35. Each component of the sample is separated in the column 35 and detected by the detector 36. The mobile phase that has passed through the column 35 is stored in the waste liquid container 23.

A detection signal from the detector 36 is transmitted to a control circuit 45, where data processing such as peak detection, peak area / height measurement, and component identification is performed. The result of the data processing is displayed on the LCD panel 121 and, if necessary, stored on a floppy disk set in the FDD 123. A program for controlling the operation of the chromatograph apparatus 10 and for performing basic data processing is stored in advance in a ROM (not shown) in the control circuit 45. The application processing program may be stored in a floppy disk and supplied to a user of the apparatus, and may be provided from the FDD 123 to the control circuit 45.

After the measurement of one sample is completed, the flow path is washed by rotating the liquid sending pump 20 at a high speed to flow a sufficient amount of the mobile phase. When removing the mobile phase container 22 from the housing 11, the liquid in the flow path is discharged to the waste liquid container 23 by switching the drain valve 15.
In addition, maintenance of the liquid sending pump 20 (exchange of a check valve or a high-pressure seal, etc.) and exchange of the column 35 are performed by the main door 12.
By opening the sub-door 13, the operation can be easily performed from the front.

In the above embodiment, a heat transfer type by block heating is used as the constant temperature unit. However, when an air circulation type is used, the door 32 of the constant temperature unit 21 is used as described above.
Instead of providing the sub door 13 separately, the door of the constant temperature unit itself may be exposed to the front of the housing 11 and a drain valve and an injector may be provided there.

[0020]

According to the liquid chromatograph of the present invention, all the elements required for analysis are housed in a single housing, so that there is no need for the user to perform wiring or piping between the elements. Easy to use. Also, since the distance between the sample injector and the column can be shortened,
Sample diffusion can be minimized, and highly accurate analysis can be performed. Further, since the data processing circuit is already provided in the present apparatus, it is not necessary to separately connect to a dedicated data processing apparatus such as a personal computer, and the installation area can be significantly reduced as compared with the conventional apparatus.

[Brief description of the drawings]

FIG. 1 is a plan view (a), front view (b), and side view (c) of a portable liquid chromatograph apparatus according to one embodiment of the present invention.

FIGS. 2A and 2B are a plan sectional view, a front view with a door removed, and a side view of the apparatus of the embodiment.

FIG. 3 is a cross-sectional view (a), a vertical cross-sectional view (b), and a front view (c) of a thermostat unit with a door removed.

FIG. 4 is a flow chart and an electric circuit diagram of the liquid chromatograph device of the embodiment.

FIG. 5 is a front view of a conventional liquid chromatograph with a data processing device.

[Explanation of symbols]

 DESCRIPTION OF SYMBOLS 10 ... Liquid chromatograph apparatus 11 ... Housing 114 ... Main door rotation axis 115 ... Main door latch button 116 ... Sub door rotation axis 12 ... Main door 121 ... LCD panel 122 ... Keyboard 123 ... Floppy disk drive (FDD) 13 … Auxiliary door 131… Valve maintenance opening 15… Drain valve 16… Injector 17… Sample loop 20… Liquid pump 21… Constant temperature unit 22… Mobile phase container 23… Waste liquid container 35… Column 36… Detector 40… Heater 43… Temperature sensor 45 ... Control circuit

Claims (1)

(57) [Claims] 1. a) a liquid sending pump for sending a mobile phase to a column; b) a constant temperature unit in which a column and a detector are disposed; and c) a liquid sending pump, a constant temperature unit and a detector. A control circuit that performs predetermined data processing based on a detection signal generated by the detector, and d) a liquid pump and a constant temperature unit are housed therein, and a space capable of housing a mobile phase container and a waste liquid container is provided. In addition to the above, an inlet for a sample injector is provided on an outer surface, and an input unit for inputting a command to the control circuit and data generated by the control circuit are displayed on an outer surface of a door that opens and closes a front opening. A liquid chromatograph apparatus comprising: a housing provided with a display unit for the liquid crystal display; and e) a pipe connecting the liquid feed pump, the sample injector, the column, and the detector.