CHROMATOGRAPH DEVICE

Abstract

A chromatograph device which makes it possible to suppress a carry-over phenomenon. A sample injection unit for collecting a liquid sample and injecting a predetermined amount of liquid sample into a mobile phase; a sample introduction tube a distal end section of which has a needle formed therein and a terminal end section of which is connected to the sample injection unit; a separation column which is coupled via a column coupling tube to the sample injection unit, and through which the mobile phase where the liquid sample has been injected passes; and a detection unit that is connected to the separation column and detects a component in the liquid sample. The column coupling tube is provided with an ultrasonic vibrator for vibrating the tube.

Claims

1-5. (canceled)

6. A chromatograph device comprising: a sample injector collecting a liquid sample and injecting a predetermined amount of liquid sample into a mobile phase; a sample introduction tube a distal end section of which has a needle formed therein and a terminal end section of which is connected to the sample injector; a separation column which is coupled via a column coupling tube to the sample injector, and through which the mobile phase where the liquid sample has been injected passes; a detector connected to the separation column and detecting a component in the liquid sample; and a cleaning mechanism including a container in which water is accommodated and the column coupling tube is immersed in the water and an ultrasonic vibrator attached to the container and removing a residual component in the column coupling tube by the ultrasonic vibrator vibrating the column coupling tube by generating ultrasonic waves.

7. The chromatograph device according to claim 6, comprising: a needle driver moving the needle; and a table where a plurality of sample containers accommodating liquid samples are placed.

8. The chromatograph device according to claim 7, comprising a controller operating the ultrasonic vibrator between liquid sample measurement and liquid sample measurement.

9. The chromatograph device according to claim 6, wherein a vibration frequency of the ultrasonic vibrator is 20 to 80 kHz inclusive.

10. The chromatograph device according to claim 6, wherein the sample injector includes a syringe pump collecting a predetermined amount of liquid sample, and a port valve interconnecting the syringe pump and the sample introduction tube or interconnecting the sample introduction tube and the column coupling tube.

Description

BRIEF DESCRIPTION OF THE DRAWINGS

[0027] FIG. 1 is a schematic configuration diagram illustrating an LC/MS as an example of a chromatograph device according to the invention.

[0028] FIG. 2 is a schematic configuration diagram illustrating the same LC/MS as in FIG. 1.

[0029] FIG. 3 is a schematic configuration diagram illustrating an example of a general LC/MS.

[0030] FIG. 4 is a schematic configuration diagram illustrating the same LC/MS as in FIG. 3.

MODE FOR CARRYING OUT THE INVENTION

[0031] Hereinafter, an embodiment of the invention will be described with reference to accompanying drawings. It is a matter of course that the invention is not limited to the embodiment described below and includes various aspects within the scope of the invention.

[0032] An LC/MS will be used as an example in the following description of a configuration example of a chromatograph device according to the invention, and a schematic configuration thereof is illustrated in FIGS. 1 and 2. The same reference numerals will be used to refer to parts similar to those of the above-described LC/MS 101 according to the related art and description thereof will be omitted.

[0033] An LC/MS 1 is provided with a mobile phase reservoir 10 storing a mobile phase, a feed pump 11 connected to the mobile phase reservoir 10, a column coupling tube (column IN side piping) 12, a separation column 13 coupled to the column coupling tube 12, a column thermostat 14 keeping the separation column 13 at a substantially constant temperature, a detector (detection unit) 15 connected to the separation column 13, an auto-sampler 20 injecting a liquid sample into the mobile phase, a controller 40 controlling the LC/MS 1, and a cleaning mechanism 50.

[0034] The controller 40 is provided with a CPU 41 and an input unit 42. To describe the functions that are processed by the CPU 41 in blocks, the CPU 41 has an auto-sampler controller 41a controlling the auto-sampler 20, an analysis controller 41b receiving an ion intensity signal from the detector 15, and a cleaning mechanism controller 41c controlling the cleaning mechanism 50. The cleaning mechanism controller 41c performs control for operating an ultrasonic vibrator 52 of the cleaning mechanism 50 after the termination of measurement of one liquid sample and until the initiation of measurement of the next liquid sample.

[0035] The cleaning mechanism 50 is provided with a container 51 accommodating water and the ultrasonic vibrator 52 attached to the container 51. The ultrasonic vibrator 52 can be attached to any place (such as the bottom surface) of the container 51 insofar as vibration can be performed. The column coupling tube 12 is immersed in the water in the container 51.

[0036] In the cleaning mechanism 50, the ultrasonic vibrator 52 generates ultrasonic waves in the water accommodated in the container 51. The ultrasonic waves generated at this time are non-coherent compression waves and vibrate the column coupling tube 12 immersed in the water by being reflected by the inner wall of the container 51. As a result, the vibration is uniformly transmitted and a residual component in the column coupling tube 12 can be effectively removed.

[0037] The vibration of the ultrasonic vibrator 52 is controlled by the cleaning mechanism controller 41c. In addition, it is preferable that the vibration frequency of the ultrasonic vibrator 52 is 20 to 80 kHz inclusive so that the standing waves of the ultrasonic waves are sufficiently generated with respect to the water accommodated in the container 51. Sufficient residual component cleaning may be impossible in a case where the vibration frequency of the ultrasonic vibrator 52 is less than 20 kHz and an increase in analysis (cleaning) time arises in a case where the vibration frequency of the ultrasonic vibrator 52 exceeds 80 kHz. In addition, it is preferable that the operating time of the ultrasonic vibrator 52 is 20 to 120 seconds inclusive so that the effect of the ultrasonic waves is obtained without an increase in analysis time.

[0038] An analysis method for automatically and continuously analyzing multiple liquid samples by using the LC/MS 1 will be described below. Firstly, the auto-sampler controller 41a of the controller 40 controls ports a to m of a flow path switching valve 33 and a flow path switching valve 34 such that the ports a to m are in the state that is illustrated in FIG. 2. Accordingly, the mobile phase supplied via the feed pump 11 from the mobile phase reservoir 10 is sent to the separation column 13 through the column coupling tube 12. Next, the auto-sampler controller 41a performs a movement such that a desired sample vial S comes directly below a needle 22a, and then inserts the needle 22a into the sample vial S by lowering the needle 22a. Then, the auto-sampler controller 41a fills a sample introduction tube 22 with the liquid sample in the sample vial S by pulling a plunger 31b of a syringe pump 31.

[0039] Next, the auto-sampler controller 41a moves an injection port 32 such that the injection port 32 is directly below the needle 22a, and then inserts the needle 22a into the injection port 32 by lowering the needle 22a. Then, the auto-sampler controller 41a controls the ports a to m of the flow path switching valves 33 and 34 such that the ports a to m are in the state that is illustrated in FIG. 1. Accordingly, the mobile phase supplied via the feed pump 11 from the mobile phase reservoir 10 is sent to the column coupling tube 12 through the sample introduction tube 22, the needle 22a, and the injection port 32. At this time, the liquid sample with which the sample introduction tube 22 is filled is sent to the column coupling tube 12 with the mobile phase, is subjected to component separation in the separation column 13, and then is subjected to sequential detection by the detector 15.

[0040] Subsequently, the auto-sampler controller 41a controls the ports a to m of the flow path switching valves 33 and 34, such that the ports a to m are in the state that is illustrated in FIG. 2, after injecting the liquid sample into the column coupling tube 12. Next, the auto-sampler controller 41a moves a rinse port 24 such that the rinse port 24 is directly below the needle 22a, and then inserts the needle 22a into the rinse port 24 by lowering the needle 22a. Then, the auto-sampler controller 41a allows the cleaning solution in a container 36 to flow into the sample introduction tube 22 by pulling and inserting the plunger 31b.

[0041] After the liquid sample measurement, the cleaning mechanism controller 41c operates the ultrasonic vibrator 52 for a predetermined time. Subsequently, the auto-sampler controller 41a performs control for measuring the next liquid sample by the same procedure as above.

[0042] In the LC/MS 1 that has the configuration according to the invention as described above, the inside of the column coupling tube 12 is reliably cleaned, and thus the occurrence of a carry-over phenomenon can be suppressed. In addition, waiting time for stabilization of the separation column 13 is unnecessary because a cleaning solution different from the mobile phase does not have to flow into the column coupling tube 12.

Another Embodiment

[0043] The above-described LC/MS 1 is configured such that the ultrasonic vibrator 52 is attached to the container 51. Alternatively, the ultrasonic vibrator 52 may be attached to the column coupling tube 12 or the ultrasonic vibrator 52 may be attached to a preheater section after the preheater section is provided.

INDUSTRIAL APPLICABILITY

[0044] The invention can be used in, for example, a liquid chromatograph device measuring multiple liquid samples.

REFERENCE SIGNS LIST

[0045] 1 LC/MS (chromatograph device) [0046] 12 Column coupling tube [0047] 13 Separation column [0048] 15 Detector (detection unit) [0049] 22 Sample introduction tube [0050] 22a Needle [0051] 30 Sample injector [0052] 52 Ultrasonic vibrator