JPH11281635A - Ion analyzing device - Google Patents

Abstract

PROBLEM TO BE SOLVED: To enable continuous measurement by using a calibration solution with higher concentration and stability than a sample and shortening the trap time of the calibration solution. SOLUTION: In the case of not being in component concentration mode, a calibration solution solenoid valve 11a is closed, and a channel valve 15 is opened. A sample from a sample tank 13 is passed from the connecting opening 5 of a switching valve 10 to a calibration solution measuring loop 10a and is discharged through a concentrating valve 4. Next, in the case of becoming in concentration mode, the concentrating valve 4 is switched, and the sample is discharged through a concentrating column 5. Concentration is performed at the rate of flow of 2 ml per minute for 10 minutes to concentrate a component to be analyzed in 20 ml of a sample. The concentrating valve 4 is switched, and an eluant stored in an eluant tank 6 is delivered by an eluant pump 7 and is flowed from the concentrating valve 4 to the concentrating column 5. The concentrated component to be analyzed is transferred to a conductivity detector 3 via a separating column 2 to measure conductivity and to determine the component to be analyzed. At the time of calibration, an eluant stored in the eluant tank 6 is transferred to the conductivity detector 3 to measure its component and concentration and to perform calibration.

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to an ion analyzer, and more particularly to an ion analyzer which prevents deterioration of a calibration liquid and shortens the calibration time of the apparatus.

[0002]

2. Description of the Related Art When an ion analyzer (for example, ion chromatography) is used continuously, a calibration solution is injected at predetermined time intervals (or as needed) to monitor whether or not the apparatus is functioning normally. I have.

[0003]

However, when analyzing at the ppt or ppb level in such an apparatus, a calibration solution having a ppt or ppb level is required. However, such a low-concentration calibration solution is difficult to maintain the stability of the concentration and components, and because of its low concentration, it is susceptible to contamination and may cause measurement errors. I needed to. Therefore, there is a problem that continuous analysis is hindered. The present invention has been made in order to solve such problems of the related art, and an object of the present invention is to provide an ion analyzer capable of performing calibration using a highly stable calibration solution having a higher concentration than a sample. I have.

[0004]

In order to achieve the object, according to the present invention, an analytical component contained in a sample is concentrated on a concentration column, and the concentrated analytical component is conveyed to a separation column with an eluent. An ion analyzer that separates the charged ion species of the target component and analyzes the components of the ion species from the separation column, wherein the sample transport means transports a fixed amount of the sample to the concentration column; And a calibration liquid transport means for transporting a small amount of the calibration liquid together with the transport liquid to the concentration column with a concentration higher than the concentration of the calibration liquid.

[0005]

When the components are concentrated, a predetermined amount of the sample is transported to the concentration column by the sample transport means. At the time of calibration, a predetermined amount of the calibration liquid having a higher concentration and a lower concentration than the predetermined amount of the sample flowing through the concentration column is transported by the calibration liquid transport means. If transported, the concentration column will trap the calibration solution in a short time. Since the predetermined amount of the sample to be passed through the concentration column and the fixed amount of the calibration solution are known, a calibration solution having a stable concentration and components can be used.

[0006]

DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS The present invention will be described below in detail with reference to the drawings. FIG. 1 is a configuration diagram showing an example of an embodiment of the present invention. In the figure, a separation column 2 and a conductivity detector 3 are stored in a thermostat 1. A concentration valve 4 is connected to one end of the separation column 2. The concentrated valve 4 has a concentration column 5. Further, an eluent pump 7 for transporting the eluent stored in the eluent tank 6 is connected to the concentrated valve 4, and a sample pump 8 for transporting the sample liquid and the calibration liquid is connected thereto.

The switching valve 10 has a measuring loop 10a for measuring the calibration liquid. The switching valve 10 is provided with a calibration liquid tank 11 storing the calibration liquid and a calibration liquid priming pump 12 via an electromagnetic valve 11a. It is connected. The switching valve 10 is connected to a sample tank 13 and a pure water tank 14 storing pure water. The drainage tank 16 stores the waste liquid of the conductivity detector 3 and the calibration liquid priming pump.

In the above configuration, when the mode is not the component concentration mode, the solenoid valve 11a is closed, and the flow path valve 15 is open on the side of the sample tank 13. Then, by starting the sample pump 8, the sample from the sample tank 13 is connected to the connection port 5 → 4 → the measuring loop 10a → 1 → 6 of the switching valve 10.
Through the connection ports 4 → 5 of the concentration valve.

Next, in the concentration mode, the concentration valve is switched, and the sample is discharged through 4 → 3 → concentration column 5 → 6 → 5. This concentration mode is performed, for example, at a flow rate of 2 ml per minute for 10 minutes to concentrate the analytical components in a 20 ml sample.

Next, the concentration valve is switched, and the eluent stored in the eluent tank 6 is sent out by the eluent pump 7 and flows through the 1 → 6 concentration column 5 → 3 → 2 of the concentration column 4. As a result, the concentrated analysis component is conveyed to the conductivity detector 3 via the separation column 2, and the conductivity is measured by the conductivity detector 3 to specify the analysis component. Conductivity detector 3
The eluate that has passed through is stored in the waste liquid tank 14.

Next, at the time of calibration, the flow path valve 15 is switched so as to pass the pure water stored in the pure water tank 14, and first, the switching valve 10 is switched from the pure water tank 14 to perform cleaning of the piping. Sample connection port 5 → 4 → Measuring loop 10a →
It passes through 1 → 6 and is discharged through the connection port 4 → 5 of the concentration valve.

After the washing, the flow valve 15 is kept open, and the pure water is kept flowing with the switching valve 10 having a flow path of 5 → 6 (solid line). At this time, the concentration valve 4
Is switched so as to be a flow path on the dotted line side.

Next, the solenoid valve 11a is opened, and the calibration liquid priming pump 12 is started. As a result, the calibration liquid stored in the calibration liquid tank 11 is sucked toward the priming pump 12 through 2 → 1 → the measuring loop 10a → 4 → 3 of the switching valve 10 and stored in the waste liquid tank 16. As a result, the calibration liquid is trapped in the measuring loop 10a. The amount of the calibration liquid to be trapped is, for example, 100 μl.

Next, the solenoid valve 11a is closed, the priming pump 12 is stopped, and the switching valve 10 is switched to the flow path of 5 → 4 → measuring loop 10a → 1 → 6 (solid line). The pure water in the tank 14 is sent to the concentration pump 4 side). As a result, the calibration liquid trapped in the measuring loop 10a is conveyed to pure water, flows into the concentration valve 4, and is discharged through the valves 4 → 3 → concentration columns 5 → 6 → 5.

In this concentration mode, the amount of water supplied from the sample valve is, for example, 2 ml per minute. In this case, after the calibration liquid trapped in the measuring loop 10a reaches the concentration column, pure water is continuously supplied, for example, for about 1 minute. It is sufficient that the calibration liquid in the flow pipe can be completely washed. As a result, the calibration liquid in 100 μl was concentrated in the concentration column 5.

Next, the concentration valve is switched in the same manner as described above, the eluent pump 7 is started, and the eluate stored in the eluent tank 6 flows from the concentration column 4 to the 1 → 6 concentration column 5 → 3 → 2. The concentrated analytical component is conveyed to the conductivity detector 3 via the separation column 2, and the conductivity detector 3 measures the component and concentration of the known component to perform calibration.

Although not shown in the drawings, the timing of starting each pump and switching each valve is performed in accordance with a sequence recorded in the CPU in advance. In the above configuration, for example, when the concentration of the measurement component contained in the sample solution is set to the ppb level, and this sample solution is passed through the concentration column at a flow rate of 2 ml / min for 7 minutes, 14 ml (14
000 μl) of the measured component is trapped. On the other hand, 100 μl of the calibration solution is transported with pure water and passes through the concentration column, but only the measurement components contained in 100 μl are trapped.

That is, the calibration liquid is 140
What is necessary is to prepare the thing of twice concentration. As a result, for example, even if the sample solution has a ppt or ppb level, a calibration solution having a high concentration or a high component stability (for example, ppm level) can be used,
An ion analyzer capable of continuous analysis can be realized. In addition, since the calibration solution is transported with pure water and trapped when it reaches the concentration column, the time for flowing the pure water may be as long as washing the pipes, and the time for trapping the calibration solution can be reduced. . Further, since the calibration liquid passes through the switching valve 10, the sample pump 8, the concentration valve 4, and the concentration column 5, it also has a check function when any one of them does not function properly.

It is to be noted that the above description of the present invention has been presented by way of explanation and illustration only of particular preferred embodiments. Thus, it will be apparent to one skilled in the art that the present invention may be modified or modified in many ways without departing from its essentials. For example, the timing of calibration, and the positions, types and numbers of pumps and valves are not limited to those in the embodiment, but may be arbitrary. Good. The scope of the present invention defined by the description in the claims section is intended to cover alterations and modifications within the scope.

[0020]

As described above, according to the present invention, a sample transport means for transporting a fixed amount of sample to a concentration column, and a sample transport means having a higher concentration than the sample every predetermined time,
In addition, since the calibration solution transport means for transporting a small amount of the calibration solution together with the transport solution to the concentration column is provided, a calibration solution having a higher concentration and a higher stability than the sample can be used, and the calibration solution trap time can be shortened. Thus, an ion analyzer capable of continuous measurement can be realized.

[Brief description of the drawings]

FIG. 1 is a configuration diagram showing an example of an embodiment of an ion analyzer according to the present invention.

[Explanation of symbols]

 Reference Signs List 1 constant temperature bath 2 separation column 3 conductivity detector 4 concentration valve 5 concentration column 6 eluent tank 8 sample pump 10 switching valve 10a measuring loop 11 calibration solution tank 11a calibration solution solenoid valve 12 calibration solution priming pump 13 sample tank 14 pure water Tank 15 Flow path valve 16 Flow path valve

Claims (3)

[Claims] An analytical component contained in a sample is concentrated in a concentration column, and the concentrated analytical component is conveyed to a separation column with an eluent to separate charged ion species of a target component. In an ion analyzer for analyzing a kind of component, a sample transport means for transporting a fixed amount of sample to the concentration column, and a concentration higher than the concentration of the sample every predetermined time, and a small amount of calibration liquid together with the transport liquid. An ion analyzer characterized by comprising a calibration liquid transport means for transporting the calibration liquid to the concentration column. 2. The ion analyzer according to claim 1, wherein said carrier liquid is pure water. 3. The ion analyzer according to claim 1, wherein the concentration of the calibration liquid has a low degree of deterioration with the passage of time.