JPH05223744A - Trace component analyzer - Google Patents

Abstract

PURPOSE:To obtain a device for analyzing a trace of constituents which can perform measurement accurately and highly sensitively even if a great amount of a sample liquid is poured by continuously mixing the sample liquid which is poured into a reaction reagent and the reaction reagent which bypasses a sample-pouring part at an exit of the sample-pouring part. CONSTITUTION:At an exit of a sample-pouring part 1, a pure water which is poured into a reaction reagent and a reaction reagent which bypasses 19 the pouring part 1 are mixed continuously. The mixed liquid is introduced to a reaction machine 4 and is subjected to mixing and reaction. Then, the liquid is cooled by a cooling coil 13 and is introduced to an absorbance meter which is used as a detector 14 for measuring absorbance, thus obtaining silicic acid ion concentration according to the peak value. Since all of the pure water which is poured in great quantity are mixed with a color-developing liquid, all of the silicic acid ion within the pure water develop color, thus achieving a normal measurement without causing a peak to be buried under a base line at a low-concentration region of the silicic acid ion or the peak to be split.

Description

Detailed Description of the Invention

The present invention relates to an apparatus for quantitatively analyzing trace components in water with high sensitivity by using, for example, a single-channel FIA (flow injection analysis method) involving a chemical reaction.

[0002]

2. Description of the Related Art FIG. 3 shows the above-mentioned trace component analyzer. In this figure, 1 is a sample injection part, which is composed of, for example, a 6-way sample injection part having 6 ports 1a to 1f. A sample liquid supply line 2, a reaction reagent supply line 3 and a reactor 4 are connected to the sample injection unit 1.

That is, the sample liquid supply line 2 is connected to the port 1a, and its upstream side is connected to a sample liquid supply source (not shown) via a pump (not shown). The reaction reagent supply line 3 is connected to the port 1d, includes a pump 5 and a deaerator 6, and the upstream side thereof is connected to the reaction reagent tank 7. Further, the reactor 4 is connected to the port 1c via the flow path 8. In addition, 9 is a sample loop connecting between the ports 1b and 1e, 10 is connected to the port 1f, and the waste liquid tank 11
It is a sample liquid discharge line equipped with. Further, 12 is a pump connected to the deaerator 6.

Reference numeral 13 is a cooling coil provided on the outlet side of the reactor 4, and 14 is a detector such as an absorptiometer.
Further, 15 is a waste liquid tank connected to the detector 14 via a back pressure coil 16, 17 is a recorder, and 18 is a data processing device. The reactor 4 and the cooling coil 13 are housed in appropriate thermostats.

In the trace component analyzer thus constructed, the sample injection unit 1 injects the sample solution into the reaction reagent, and both of them are mixed and reacted in the reactor 4, and a quantity is quantified in the detector 14. By doing so, it is possible to quantitatively analyze the trace components contained in the sample liquid.

[0006]

However, a large amount of sample liquid (for example, 500 μm) is added to the above trace component analyzer.
When the sample is injected into l) for analysis, an unreacted part is formed because a part of the injected sample liquid is not mixed with the reaction reagent. In the resulting chromatogram, the peak may be buried in the baseline or the peak might be broken in the low concentration region of the target component, and normal measurement could not be performed.

The present invention has been made with the above matters in mind, and the purpose of the invention is
An object of the present invention is to provide a trace component analyzer that can perform normal measurement even when a large amount of sample liquid is injected, and can measure with high sensitivity.

[0008]

In order to achieve the above object, in the present invention, at the outlet side of a sample injection part for injecting a sample solution into a reaction reagent, a sample solution injected into the reaction reagent is used. , And the reaction reagent bypassing the sample injection part are continuously mixed.

[0009]

According to the above construction, all of the sample liquid injected in large quantity is mixed with the reaction reagent, so that there is no unreacted portion. As a result, in the low concentration range of the target component, the peak is not buried in the baseline and the peak is not broken, and normal measurement can be performed.

[0010]

Embodiments of the present invention will be described below with reference to the drawings. In the following description, the same parts as those shown in FIG. 3 are the same parts.

FIG. 1 shows an example of a trace component analyzer according to the present invention. The difference between this trace component analyzer and the conventional one shown in FIG. 3 is that the sample injection part 1 is bypassed. The reaction reagent supply line 3 and the flow path 8 on the downstream side of the sample injection part 1 are connected by a bypass line 19.

Next, the case of quantifying silicate ions in, for example, ultrapure water in the trace component analyzer thus constructed will be described. In this case, a sulfuric acid-acidifying color developing solution containing ammonium molybdate is used as a reaction reagent. Then, the reaction reagent is degassed by the deaerator 6, and then a constant flow rate is supplied to the reaction reagent supply line 3 by the pump 5.

On the other hand, the sample liquid supply line 2 is operated by switching the 6-way switching valve as the sample injection unit 1.
Pure water supplied by is injected into the reaction reagent supplied by the reaction reagent supply line 3. At this time, the reaction reagent flowing through the reaction reagent supply line 3 continuously flows through the bypass line 19 on the outlet side of the sample injection unit 1.

Therefore, on the outlet side of the sample injection part 1, the pure water injected into the reaction reagent and the sample injection part 1
Is continuously mixed with the reaction reagent bypassed. The mixed liquid is introduced into the reactor 4 and mixed / reacted. Then, after being cooled by the cooling coil 13, this liquid is introduced into an absorptiometer as a detector 14 to measure the absorbance, and the silicate ion concentration is obtained from the peak value.

According to the above-described embodiment, since a large amount of pure water injected is mixed with the color-developing liquid, all silicate ions in the pure water develop color. As a result, the peak is not buried in the baseline or the peak is not broken in the low concentration region of silicate ions, and the measurement can be normally performed. Therefore, if a large amount of sample liquid is injected, highly sensitive measurement can be performed. According to an experiment conducted by the inventor, it was found that the measurement can be normally performed even if a sample solution of about 10 times (5 ml) as compared with the conventional one is injected.

FIG. 2 shows another embodiment of the present invention. In this embodiment, instead of the bypass line 19, the reaction reagent supply line 3 is branched on the upstream side of the deaerator 6. A second reaction reagent supply line 20 is provided in parallel with the reaction reagent supply line 3, and a deaerator 21, a pump 22, and a mixing joint 23 are sequentially provided from the upstream side of the second reaction reagent supply line 20, and the port of the sample injection unit 1 is provided. 1c is connected to the inlet side of the mixing joint 23. It is needless to say that the same effect as that of the above embodiment can be obtained even in the case of such a configuration.

Needless to say, the present invention can be widely applied to other than the quantitative analysis of silicate ions contained in pure water.

[0018]

As described above, according to the present invention,
Even if a large amount of sample solution is injected, the peak will not be buried in the baseline or the peak will not be broken in the low concentration range of the target component, and normal measurement can be performed and highly sensitive measurement can be performed. It became so.

[Brief description of drawings]

FIG. 1 is a diagram schematically showing a configuration example of a trace component analyzer according to the present invention.

FIG. 2 is a diagram schematically showing another configuration example of the trace component analysis device according to the present invention.

FIG. 3 is a diagram schematically showing a configuration of a conventional trace component analyzer.

[Explanation of symbols]

DESCRIPTION OF SYMBOLS 1 ... Sample injection part, 3 ... Reaction reagent supply line, 4 ... Reactor, 14 ... Detector.

Claims (1)

[Claims] 1. A reaction reagent supply line and a reactor are connected to a sample injection part so that a sample solution is injected into the reaction reagent from the sample injection part, and at the outlet side of the reactor. In a trace component analyzer connected to a detector, on the outlet side of the sample injection section, the sample solution injected into the reaction reagent and the reaction reagent bypassing the sample injection section are continuously mixed. A trace component analyzer characterized in that