JPH0634614A - Liquid chromatograph - Google Patents

Abstract

PURPOSE:To improve analysis precision and reduce the required space for installation by shortening the piping length between the injector in an autosampler and the column of a permanent temperature bath, these constitute a liquid chromatograph, and installing multiple injectors for realizing the function obtained with multiple autosamplers. CONSTITUTION:A sample is injected into an injector 20 through a syringe 26 and then moved to a column 19 assigned in a permanent temperature bath 4, the titled liquid chromatograph is thus configured. An autosampler 21 provided with a syringe 26 which attracts/injects the sample while moving between a sample staring vessel 25 and the injector 20, internally assigned, is provided. The autasampler 21 is assigned on the permanent temperature bath 4 and a partition wall 22 for partitioning them is provided with the injector 20, placed near the column 19, and further, a valve head 20a of the injector 20 is assigned within the permanent temperature bath 4.

Description

Detailed Description of the Invention

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention shortens the piping between the injector in the autosampler and the column in the thermostatic chamber to improve the analysis accuracy, and installs a plurality of injectors to provide a plurality of autosamplers. The present invention relates to a liquid chromatograph capable of reducing the installation area of the liquid chromatograph.

[0002]

2. Description of the Related Art A conventional autosampler uses a cylinder for measuring a sample or a special valve for injecting a sample to inject a sample into a column.
However, in this method, the pipe between the cylinder and the special valve becomes long, the dead volume increases, which promotes the waste and diffusion of the sample, and the cylinder can be used for measuring a large volume of washing liquid in addition to the sample. Since the cylinder was used, the capacity of the cylinder was inevitably increased, the accuracy of measurement was lowered accordingly, and an injection error was likely to occur, and there was a problem that data with good reproducibility could not be obtained.

In particular, when a microcolumn or the like requiring a minute amount of injection is used, the injection amount becomes 1 μl or less, and it has been very difficult to obtain the absolute amount and reproducibility of the injection amount. Therefore, the autosampler has a small dead volume and can secure the absolute amount of injection,
Moreover, it is required to obtain data with good reproducibility and to be compact and lightweight.

When a liquid chromatograph is equipped with such an autosampler, for example, Japanese Examined Patent Publication No. 3-63707.
With reference to the publication, a pump constituting a mobile phase liquid sending device,
A method is conceivable in which the autosampler and the thermostat are juxtaposed next to each other and connected with each conduit.

[0005]

However, in this case, the pipe between the injector valve provided in the autosampler and the column in the constant temperature bath becomes long, the dead volume becomes large, and the pipe is moved. There is a problem that the diffusion of the sample is promoted, the peak width of the chromatogram is widened, and a large installation area is required to install the related equipment.

The present invention solves such a problem, shortens the pipe length between the injector provided in the autosampler and the column arranged in the constant temperature bath, and suppresses the diffusion of the sample moving in the relevant portion to improve the analysis accuracy. It is an object of the present invention to provide a liquid chromatograph capable of improving the performance and reducing the installation area of the equipment.

[0007]

Therefore, the liquid chromatograph of the present invention is a liquid chromatograph in which a sample is injected into an injector through a syringe and the sample is moved to a column arranged in a thermostatic chamber. , An autosampler equipped with a syringe that moves between the sample storage container and the injector placed inside and aspirates and injects the sample is placed at the top of the thermostat, and the autosampler and thermostat are placed. In the partition wall that divides the, the injector is arranged in close proximity to the column, the valve head part of the injector is arranged inside the thermostat, and the injector provided in the autosampler and the column inside the thermostat By shortening the pipe length, suppressing the diffusion of the sample moving in the relevant section, improving the analysis accuracy, and It is characterized in that so as to achieve a small space of the location area. Further, the syringe and the injector are configured to have a small volume so that a small amount of sample can be accurately measured and the absolute amount of the injected amount can be easily and accurately obtained.
Further, it is characterized in that a plurality of injectors are provided so as to face the auto sampler so that a plurality of auto samplers can be obtained with one sampling device.

[0008]

[Operation] Since the autosampler equipped with a syringe for moving the sample storage container and the injector placed inside to inject the sample by suction is provided, the sample introduction part in the liquid chromatograph can be fully automated. Since the auto sampler is placed above the constant temperature bath, the installation area can be reduced compared to the case where these are placed side by side.
Since the injector is placed close to the column on the partition wall that divides the autosampler and the constant temperature chamber, the length of the conduit connecting the column and the injector can be shortened, and the diffusion of the sample moving in the part is suppressed. it can. Since the valve head portion of the injector is arranged inside the constant temperature bath, the temperature difference between the sample and the constant temperature bath becomes small, and a good separation state on the column can be obtained. Since the syringe and the injector are configured with small volumes, a minute amount of sample can be accurately measured, and the absolute amount of the injection can be easily and accurately obtained. Since a plurality of injectors are provided so as to face the auto sampler, a plurality of auto samplers can be obtained with one sampling device, which can be manufactured at low cost and the installation space can be greatly reduced.

[0009]

DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS An illustrated embodiment arranged for high pressure gradient analysis using the present invention will be described below. In FIG. 1, 1 is a liquid chromatograph systematically arranging each instrument functionally. A detector 3 and a constant temperature bath 4 are arranged adjacent to each other on the floor surface 2. Of these, a liquid feeding device 7 having a pair of liquid feeding pumps 5 and 6 built in on the detector 3,
Carrier reservoir 1 in which two eluent bottles 9 and 10 are arranged on the upper liquid sending device 8
1 is arranged.

On one side of the detector 3, the liquid feeding devices 7 and 8, and the carrier reservoir 11, there are provided operation parts 3a, 7a, 8a and 11a each having an input key and a display part.
The front of the constant temperature bath 4 can be opened and closed by a pair of doors 12 and 13, and one door 13 is provided with two manual injectors 14 that can inject a sample from the outside. In the figure, 14a is a rotary operation knob.

Inside the constant temperature bath 4, a pair of switching valves 1
5 and 16 are arranged vertically or horizontally, and two columns 17 and 18 are arranged between them in a vertically separated manner,
Their ends can be connected to the switching valves 15 and 16 via connecting conduits (not shown). The column 17,
A common column 19 is vertically arranged near the position 18, and its upper end is connected to the injector 20 and its lower end can be connected to the detector 3 through a connecting conduit (not shown).

In the case of the embodiment, the injector 20 is 1
A small capacity manual injector of μ to 10 μl or less is used, which is located directly above the upper end of the regular column 19 in the partition wall 22 that divides the constant temperature bath 4 and the autosampler 21 that is detachably arranged on the constant temperature bath 4. It is mounted in a standing position, the inlet side is exposed to the inside of the auto sampler 21, and the valve head portion 20a of the injector 20 located below is located above the inside of the thermostatic chamber 4.

In the case of the embodiment, the injector 20 is 1
What is used for a manual injector of μ to 10 μl or less is used, a rack 24 is provided in the lower part of the auto sampler 21, and a plurality of sample storage containers 25 for storing a sample solution are stored in the rack 24. A syringe 26, which is a sample-only scale, is movably provided above the.

In the case of the embodiment, the syringe 26 is 1 μ to 1 μm.
A small volume of 0 μl or less, which can be manually operated, is used.
5 is waited above, and at the time of sample injection, the sample is moved directly above a predetermined sample storage container 25, and then moved downward to position the injection port in the container 25, and a predetermined amount of a predetermined amount is supplied through the suction operation of the plunger 27. Aspirate the sample.

After the sample is sucked, the syringe 26 moves upward, and when it moves a predetermined height, it horizontally moves above the injector 20 and then moves downward to insert it into the injection port of the injector 20 and eject the plunger 27. After injecting the sample through, move upward. The syringe 26 is automated for such a series of sequence operations, and these operations can be set by the operation unit 30 including the input key 28 and the display unit 29.

In addition, reference numeral 31 in the drawing denotes a cleaning adapter, 32
Is a cleaning port communicating with the waste liquid, and is connected to a waste liquid storage container (not shown) via a conduit (not shown). Reference numeral 33 is a gradient mixer provided in the constant temperature bath 4, 34 is a column provided at the other end of the constant temperature bath 4, one end of which can be connected to the manual injector 14.

2 and 3 show another embodiment of the present invention, in which the same reference numerals are used for the components corresponding to those of the above-mentioned embodiment. Among them, the embodiment shown in FIG. 2 is provided with two injectors 20 in one thermostat 4, and the common columns 19 and 19 are connected to the injectors 20 via connecting conduits, and the columns 19 and 19 are used as detectors. It is connected to 3,3. Further, the detectors 3 are installed on both sides of the constant temperature bath 4, and the liquid feeding devices 7 and 8 and the carrier reservoir 11 are arranged on them.

That is, this embodiment can be used as two autosamplers by injecting the sample into each injector 20 separately from one sampling mechanism according to the setting of the control program, and at the same time, the parallel processing of two analyzes can be performed. Will be possible. Moreover, it is cheaper than installing two auto samplers, and the installation space can be greatly reduced.

The embodiment shown in FIG. 3 is characterized in that the lower constant temperature bath 4 is removed and a pedestal 35 is attached to the relevant part so that the autosampler 21 can be used alone.

The liquid chromatograph constructed as described above comprises a detector 3, liquid feeding devices 7 and 8, a carrier reservoir 11, a constant temperature bath 4, and an autosampler 21, and is sent onto the detector 3. The liquid devices 7 and 8 are arranged vertically, and the carrier reservoir 11 is arranged on the upper liquid feeding device 8.
Further, the auto sampler 21 is arranged on the constant temperature bath 4 and integrated to form a system. Therefore, as compared with the case where the constant temperature bath 4 and the auto sampler 21 are arranged side by side, the installation space of the system can be made compact.

Further, according to the present invention, a partition wall 22 for partitioning the injector 20 into the constant temperature bath 4 and the auto sampler 21 is provided.
In the above, since the column 19 and the injector 20 are arranged at the upper end of the common column 19, that is, at the position immediately above the upstream side.
When connecting and by using a connection conduit (not shown), the connection conduit is shortened as compared with the case where the constant temperature bath 4 and the autosampler 21 are juxtaposed as described above.

Therefore, since the inside volume of the pipe is reduced due to the shortening of the conduit, the sample injected into the injector 20 moves to the column 19 with minimal diffusion when moving through the conduit. Therefore, the separation is rapidly performed while moving through the stationary phase of the column 19, and a chromatogram with a sharp peak can be obtained.

Moreover, since the syringe 26 used in the present invention is dedicated to measuring a sample and has a small volume of 1 μ to 10 μL or less, it can accurately measure a small amount of sample and the injector 20 can measure 1 μ to 1 μL. 10
Since it has a small volume of less than μl, it is possible to easily and surely obtain the absolute amount of a small amount of injected sample, and in combination with the above, obtain reproducible data.

In the case of injecting a sample having a capacity larger than that of the syringe 26, it is possible to reciprocate the syringe 26 many times to inject the sample without changing the syringe 26 and switch the injector 20 to operate. By doing so, a large amount of injection can be accepted.

In this case, the sample storage container 25 and the injector 20 in the auto sampler 21 are arranged close to the constant temperature bath 4, and the valve head portion 20a of the injector 20 is arranged to face the constant temperature bath 4. Since the temperature difference before and after the injection of the sample is made as small as possible, the sample injected into the injector 20 is maintained at a substantially constant temperature in the column 19 without being affected by the temperature difference. It migrates and promotes separation under good separation conditions.

In addition, the injector 20 includes a sample storage container 25 and a syringe 26 in the auto sampler 21.
Since it is close to the moving area of the sample, the suction and injection operation of the sample by the syringe 26 can be performed smoothly and efficiently, and the sample introducing part in the liquid chromatograph can be fully automated.

[0027]

As described above, the liquid chromatograph of the present invention is provided with an autosampler equipped with a syringe that moves between a sample storage container disposed inside and an injector to suck and inject a sample. It is possible to realize complete automation of the sample introduction unit in the chromatograph. Further, according to the present invention, since the auto sampler is arranged in the upper part of the constant temperature bath, the installation area of the equipment can be reduced as compared with the case where these are arranged side by side. Moreover, the partition wall that separates the autosampler and the constant temperature bath is provided with the injector in close proximity to the column, so that the conduit connecting the column and the injector can be shortened, and the diffusion of the sample moving in the part can be achieved. It is possible to suppress the peak broadening in the chromatogram and improve the analysis accuracy. Further, according to the present invention, since the valve head portion of the injector is arranged inside the thermostat, the temperature difference between the sample and the column becomes small, and there is an effect that a good separation state in the column can be obtained. Therefore, by constructing the syringe and the injector with a small volume, a minute amount of sample can be accurately measured, and the absolute amount of the injection amount can be easily and accurately obtained. You can get good data. Also, by providing multiple injectors facing the autosampler, multiple autosamplers can be obtained with one sampling mechanism, multiple analyzes can be processed in parallel, and the installation space for the equipment can be greatly reduced. Has the effect of.

[Brief description of drawings]

FIG. 1 is a front view showing an embodiment of the present invention in which a door on one side of a constant temperature oven is opened.

FIG. 2 is a front view showing a main part of another embodiment of the present invention, in which a door on one side of the constant temperature oven is omitted.

FIG. 3 is a front view showing a main part of still another embodiment of the present invention.

[Explanation of symbols]

 1 Liquid Chromatograph 4 Constant Temperature Tank 19 Column 20 Injector 21 Auto Sampler 22 Partition Wall 20a Valve Head 25 Sample Storage Container 26 Syringe

 ─────────────────────────────────────────────────── ─── Continuation of the front page (72) Inventor Hisashi Nishi Nishi 237-2 Sayamagahara, Iruma City, Saitama GL Sciences Co., Ltd. Musashi Factory

Claims (3)

[Claims] 1. In a liquid chromatograph in which a sample is injected into an injector via a syringe and the sample is moved to a column arranged in a thermostatic chamber, the sample is moved between the sample storage container and the injector arranged inside. do it,
An autosampler equipped with a syringe for injecting a sample is provided, the autosampler is arranged at the upper part of the thermostat, and a partition wall separating the autosampler and the thermostat is placed in proximity to the column with an injector. A liquid chromatograph characterized in that a valve head portion of the injector is arranged inside a thermostatic chamber. 2. The liquid chromatograph according to claim 1, wherein the syringe and the injector have small volumes. 3. The liquid chromatograph according to claim 1, wherein a plurality of injectors are provided so as to face the autosampler.