JPS5987359A - Concentrating type apparatus for quantitative analysis of ionic species - Google Patents

Abstract

PURPOSE:To determine a concentrating quantity of a liquid to be measured by providing a change-over valve changing over or connecting alternately a condensing column to an eluate flow path and the measuring liquid flow path, a timer controlling the driving and a pump holding the measuring liquid flow rate to a prescribed value. CONSTITUTION:A quantiative pump 3 begins the driving by command from the timer 5, and the change-over valve 1 is changed over after T hour. Thus the quantity to be measured corresponding to a product of a flow rate U and the time T predetermined respectively to the pump 3 and the timer 5 is condensed by the condensing column 2, and the measuring liquid is transported with the eluate to a seperation column 11. The aimed charge ion species in the measuring liquid is separated at the column 11, and the eluate thereat is sent to a suppressor 12b. The ion exchange is performed at the suppressor, and the background in the detection of aimed charge ion is decreased. Then a conductivity of the liquid is detected at a detector 13 and the charge ion species is analyzed quantitatively. As the result, trace concn. ion species and high concn. ion species can be analyzed exactly by one quantitative analyzer.

Description

DETAILED DESCRIPTION OF THE INVENTION The present invention provides a method for collecting at least one target charged ion species that is paired with at least one oppositely charged ion species coexisting in the sample solution by concentrating and collecting a predetermined amount of a sample liquid. This invention relates to a concentrated type ion species quantitative analyzer for stationary chromatographic analysis.

In a conventional example of such an analyzer, a concentration column filled with ion exchanger JIA II fat is attached to the sample loop part of the sample liquid sampling device, and the sample liquid injected loosely with a syringe is turned into -. Ion chromatographs are known that are configured to concentrate with a concentration column.

However, in the conventional example described above, the inner diameter of the concentration column is several mrn and the length is several cm, whereas if a syringe with an internal volume of imeO is used, only a trace amount of the target charged ion species is present in the liquid to be measured. If it is not included, there is a drawback that the liquid to be measured must be injected with a syringe several dozen times into the loose sample. However, as the number of injections of the liquid to be measured increases, the possibility that impurities or the like will be mixed into the liquid to be measured increases accordingly, which ultimately reduces the reliability of the analysis results. Furthermore, in order to inject a large amount of the liquid to be measured at once, a syringe with a large internal volume is required, and the diameter of the syringe usually increases accordingly. For this reason, the resistance when injecting the test liquid into the concentration column using the syringe increases.
Another drawback was that the injection operation was difficult.

The present invention has been made in view of these drawbacks, and its purpose is to easily and accurately determine the target charged ion species even when the target charged ion species is contained in a very small amount in the liquid to be measured. An object of the present invention is to provide a concentrated type ion species quantitative analyzer that can be used for analysis.

The present invention is characterized in that a concentrated ion species quantitative analyzer includes a switching valve that alternately switches and connects a concentrated column to an eluent flow path and a measured liquid flow path, and a timer that controls driving of the switching valve. A metering pump is provided to maintain the flow rate of the liquid to be measured in the liquid to be measured flow path at a predetermined value, and the concentration amount of the liquid to be measured is determined by the product of the flow rate and time set respectively by the metering pump and the timer. It's what I did.

(Hereinafter, the present invention will be explained in detail with reference to the drawings. The drawings are explanatory diagrams of the configuration of the embodiments of the present invention, and in the drawings, 1 has the first to sixth connection ports 1a to 1f; 1. Third and fifth
The connection ports 1a, lc, and le of the 2nd and 4th ports respectively. and the sixth connection ports 1b, 1 (1, if) are connected to the first state (solid line connection state in the figure) and the sixth connection ports 1t, xb, fa are connected to the second and fourth connection ports 1t, xb, fa, respectively. The second
2 is a column filled with a predetermined ion-exchange resin or the like and concentrates the sample to be measured; 3 is the sample to be measured;
4 is an actuator that rotates the shaft of the switching valve 1 to alternately switch between the first and second states, and 5 is a switching valve via the actuator 4. This is a timer that controls the drive of 1 and keeps the time T during which the liquid to be measured flows through the concentration column at a desired value. In addition, switching valve 1° concentration column 2. Metering pump 3. The actuator 4° and the timer 5 often constitute an automatic concentration device 6. Furthermore, 7 is a liquid pump that pumps the eluent (EL) at a predetermined flow rate (4), 8 is a damper that prevents pulsation of the eluent that is force fed by the liquid feed tube 7, and 9 is a corresponding pump. A pressure gauge 10 for measuring the pressure of the eluent has first to sixth connection ports 10a to 10f and performs the same operation as the switching valve 1 (i.e., the solid line connection state and the broken line connection state are alternately switched). A sample injector 11 is a separation column filled with a predetermined ion exchange resin and separates the target charged ion species in the liquid to be measured; 12 is an ion exchange membrane 12a which doubles the interior into a first chamber 12b and a second chamber 12c; 13 is a detector for detecting, for example, the conductivity of the liquid flowing from the first chamber +2b to quantify the target charged ion species in the liquid to be measured; 14 is a second chamber; 1
2c is a prescribed scavenger liquid (Scavenger;
This is a liquid pump that pumps SV) at a predetermined flow rate.

Still, in many cases, these components 7 to 14 constitute a standard type ion species quantitative analysis device (for example, an ion chromatography analyzer).

In the embodiment of the present invention having the above configuration, the switching valve 1
．． and the sample injector 10 are both initially kept in the first state (i.e., solid line connection state). In this state,
The liquid to be measured flows through the metering pump 3 → the fifth and sixth connection ports 1e of the switching valve 1, 1f −+ concentration column 2 → the third and fourth connection ports 1c of the switching pulp 1, and the ldO flow path. In addition, the eluent flows in the flow path from the liquid supply pump → the chamber 12b → the detector 13, and the second chamber 12 of the suppressor 12
Scavenger liquid flows through the liquid supply pump 14 through c. Next, the switching valve 1 is switched to the second state (that is, the broken line connected state) after a time T after the metering pump 3 starts driving according to a command from the timer 5. In this state,
Second and first connection ports 10 of sample injector 10
b. The eluent that has passed through 10a passes through the first and sixth connection ports 1a of the switching valve 1, if→concentration column 2→the third and second connection ports 1c, lb of the switching valve 1, and then enters the separation column 11. come to reach. Therefore, the flow rate V set in the metering pump 3 and the timer 5, respectively.
The edge of the measurement liquid corresponding to the product VT of time T and time T is concentrated in the concentration column 2, and the measurement liquid is carried by the eluent and reaches the separation column 11. In addition, target charged ion species (for example, anions) in the liquid to be measured are separated in the separation column 11, and the separation column 11
The eluate of No. 1 reaches the first chamber 12b of the suppressor 12. At 4 degrees in the suppressor, ion exchange of oppositely charged ions (for example, cations) is performed between the fluid in the first chamber 12b and the scavenge liquid in the second chamber 12c via the ion exchange membrane 12a.
The pack ground required for detecting the target charged ion species in the liquid to be measured is significantly reduced. Thereafter, the fluid in the first chamber 121] reaches the detector 13, and the target charged ion species is quantified by detecting the fluid, for example, 40% of the fluid. The sample injector 1o is used as a so-called injection-type normal switching valve in which the liquid to be measured is injected from the fifth connection port 10e using a microsyringe, etc., and is used to concentrate and quantify the liquid to be measured. It may be removed if it is only for analysis. However, the present invention is illustrated in a non-limiting example, and the sample injector 1
A plurality of automatic concentrators 6 may be connected in series between 0 and the separation column 11 to quantitatively analyze a plurality of liquids to be measured sequentially (or arbitrarily). Furthermore, a sequencer may be used instead of the timer 5 so that the injection time T of the liquid to be measured, the analysis time, etc. can be changed every time.

According to the embodiment of the present invention as described in detail above, since the liquid to be measured is introduced into the concentration column 2 by the metering pump 3, impurities etc. are more likely to be mixed into the liquid to be measured at the time of introduction compared to the conventional example. The advantage is that the chances are drastically reduced. In addition, since the concentration amount of the liquid to be measured in the concentration column 2 is configured to correspond to the product VT of the flow rate V and time T set in the metering pump 3 and timer 5, respectively, in the case of the conventional example, This has the advantage of significantly improving workability and reproducibility. Furthermore, timer 5 (or sequencer)
By setting the time according to the method, there is an advantage that the liquid to be measured can be concentrated and the target charged ion species can be quantitatively analyzed continuously. In addition, it is also possible to manually inject the liquid to be measured using the non-pump injector 10, so the switching valve 1 is used for analysis of trace concentrated ion species, and the sample injector 1 is used for analysis of high concentration ion species.
By using 0, there is an advantage that trace concentration ion species and high concentration ion species in the liquid to be measured can be quickly and accurately analyzed with one quantitative analyzer.

[Brief explanation of drawings]

The figure is a configuration explanatory diagram of an embodiment of the present invention. 1... Switching valve, 2... Concentration column, 3... Metering pump, 4... Actuator, 5... Timer,
6...Automatic concentrator, 7.14...Liquid pump, 8
... Damper, 10 ... Sample injector, 1
1... Separation column, 12... Suppressor, 13...
·Detector.

Claims (3)

[Claims] (1) The concentrated test liquid is transported to a separation column using an eluent to separate target charged ion species, and the eluate from the separation column is guided to a predetermined suppressor to perform ion exchange of oppositely charged ion species. In an apparatus for conducting chromatographic quantitative analysis of the target charged ion species by guiding the eluate from the sabre or sukara to a predetermined detector, the eluent and the liquid to be measured are connected to a concentrating column for concentrating the liquid to be measured. a switching valve that is alternately switched and connected to each flow path, a timer that controls the driving of the switching valve so that the time T during which the liquid to be measured flows through the concentration column becomes a desired value; A concentration type comprising a metering pump that maintains the flow of the passage at a predetermined flow rate V, and configured such that the concentration amount of the liquid to be measured is determined by the product VT of the time T and the flow rate V. Ion species quantitative analyzer. (2) having m1 to sixth connection ports; Third. and a fifth connection port respectively. 4th. and the first state communicated with the sixth connection port, and the sixth state and the second state communicated with the sixth connection port, respectively. and a second state in which the concentrating column is connected to the third and sixth connection ports, and the first and second connection ports are in communication with the eluent. Quantification of concentrated ionic species according to claim 1, wherein the switching valve is configured such that the switching valve is connected to a flow path and the fourth and fifth connection ports are connected to the liquid flow path. Analysis equipment. (3) A plurality of the switching valves are connected in series to the eluent flow path so that a plurality of liquids to be measured are sequentially analyzed. 2) The concentrated ionic species quantitative analyzer described in section 2).