JPS60209148A - Hermetic circulation chamber for icp analysis - Google Patents

Abstract

PURPOSE:To use the whole of a sample liquid to analysis by atomizing again the atomized sample liquid which falls in the form of a drop without arriving at a torch. CONSTITUTION:A carrier gas introduced from a carrier gas introducing part 24 of a nebulizer N is discharged from a discharge hole 26. A sample liquid 24 is sucked in this stage into a sample liquid sucking part 25 and is discharged in the form of a mist from the hole 26. Only the mist-like sample liquid 27 having a suitable size is introduced by a carrier gas into a torch port 23 by the selecting action with a mist of a chamber 21. The liquid 27 of the size except said size sticks on the inside surface of the chamber 21 and flows down in the form of a drop. The large liquid 27 falls as it is and is joined with the liquid 27 on the base of the chamber 21. The joined liquid 27 is sucked from the part 25 by the carrier gas and is discharged again in the form of a mist from the hole 26. The circulation operation is thus continued. The whole of the liquid 27 in the chamber 21 is used for analysis.

Description

DETAILED DESCRIPTION OF THE INVENTION (A) Field of Industrial Application The present invention relates to a closed circulation chamber for introducing a liquid sample used in emission spectroscopic analysis using ICP (high frequency induced plasma).

(b) In emission spectroscopic analysis using conventional technology ICP as a light source, 300
A high-frequency current with a frequency of MHz or less is passed through the coil, and discharge is caused by an electric field generated by electromagnetic induction due to time changes in the high-frequency magnetic field.1. A sample in the form of mist is introduced into the holes formed in the plasma generated by the discharge to excite it, and the wavelength and intensity of the light emitted at that time is measured with a spectrometer for qualitative and quantitative analysis of the sample. Do the following.

Regarding the conventional ICP emission spectrometer of this type, the first
This will be explained with reference to the figures.

In the figure, 1 is a sample container, and this container 1 is filled with a sample liquid 2 in which a sample is dissolved. A tube 3 connects the nebulizer N and the sample container 1.

The nebulizer N has a sample liquid introduction hole 4, a carrier gas introduction hole 5, and a sample liquid 2 that is fed by the introduced carrier gas.
A discharge port 6 through which the liquid is discharged in the form of a mist is provided. Reference numeral 7 denotes a chamber constructed by Renz-Kussgaras, which includes a torch port 7a integrally constructed with the chamber 7, a discharge portion 7b for the atomized sample liquid 2 that is not introduced into the torch port 7a, and a large diameter It has an opening 7c. The opening 7C is hermetically closed by a holder 8, and the nebulizer N is fitted into the holder 8 in an airtight manner. Reference numeral 9 denotes an inner tube similarly made of Pyrex glass, which is connected to the chamber 7.

A tube 10 is connected to the discharge part 7b of the chamber 7,
The other end of the tube 10 is connected to a pipe provided on the bottom of the sub-tank J1, and water is stored in the sub-tank 1 and the tube 10. This water is
The carrier gas and atomized liquid samples 2 and 16 introduced into the inner tube 9 from the discharge hole 6 are connected to a torch made of quartz, and the torch is connected to a torch port 7a. A coil 16 is wound and a plasma light source 17 is generated.

To explain the operation of the device configured in this way,
The carrier gas introduced into the carrier gas introduction hole 5 causes the sample liquid 2 in the sample container 1 to be introduced into the nebulizer N via the tube 3 and the sample liquid introduction hole 4, and is discharged as a mist. It is discharged from the hole 6 into the inner tube 9 of the chamber 7 . Anything other than the atomized sample liquid 2 of a size suitable for being introduced into the torch 15 via the torch port 7a falls into the inner tube 9 or adheres to its inner surface, or adheres to the inner wall of the chamber 7. The water flows down in the form of droplets and is combined with the water present in the discharge section 7b. An amount of the sample liquid 2 combined with water flows out from the sub-tank 11 into the waste liquid container 13 through the tube 12, and the waste liquid container 13 is filled with a mixed liquid 14 of water and the sample liquid.

As described above, in the chamber 7, only the atomized sample liquid 2 having an appropriate size is selected and introduced into the torch 15, and the atomized sample liquid 2 having other sizes is introduced into the tube 10. Since the sample liquid is combined with water and discarded outside, only about 5% of the sample liquid is actually effectively used for analysis, and the other 95% is wasted. Moreover, in the analysis of biological samples, the amount to be collected is very small, so in order to use this in an ICP emission spectrometer, a large amount of biological samples must be collected, resulting in the inconvenience of errors.

Also, all of the sample liquid 2 in the sample container 1 is in the Nepurizer N.
After the sample container 1 is introduced, air is introduced, which causes the plasma to disappear, so there is the inconvenience of having to be careful not to empty the sample container 1 at all times during analysis. there were.

(c), Purpose The present invention solves the drawbacks of the prior art as described above.The present invention is aimed at solving the above-mentioned drawbacks of the prior art. An object of the present invention is to provide a closed circulation chamber for ICP analysis in which the entire sample liquid can be used for analysis by denucleating the circulation that atomizes the sample liquid again.

2), Structure The present invention has a chamber with a sealed structure, turns the sample liquid in the chamber into a haze-like substance using a nebulizer, introduces this into a torch, and converts the unintroduced atomized sample liquid into a liquid sample. By performing a circulation in which the liquid is combined with the liquid and atomized again, all of the multi-sample liquid can be consumed for analysis.

(e) Embodiment An embodiment of the closed circulation chamber for ICP analysis of the present invention will be described with reference to FIG.

In the figure, reference numeral 21 denotes a spherical sealed chamber made of Pyrex glass, and is provided with a torch date 23 and a sample liquid introducing section 21g.

A nebulizer N is provided in the chamber 2, and this nepurizer N includes a carrier gas introduction part 24, a sample liquid suction part 25, and a discharge hole 26 for discharging atomized sample liquid. The carrier gas introducing portion 24 is maintained in an airtight state and protrudes to the outside through the chamber 2. In addition, the nepurizer N is provided to be located at the center of the chamber 21, and is connected to the lower end surface of the sample liquid suction section 25 that sucks the sample liquid 27 in the chamber 2, and to the inner surface of the chamber 2 facing this. The interval between is approximately 0.
It is set to be 3 to 0.5 m.

The torch port 23 is provided at a position offset with respect to the discharge hole 26 of the nebulizer N so as not to be disposed facing the discharge hole 26. The reason for this positional relationship is that the atomized liquid samples 27 of various sizes discharged from the discharge hole 26 of the Nepurizer N are directly introduced into the torch via the torch port 23 and analyzed. In order to prevent a drop in analysis accuracy, the atomized sample liquid 27 of an appropriate size can be selected in the chamber 2, avoiding a position facing the discharge hole 26 of the nebulizer N and deviating from the position. This is because the above-mentioned selection effect can be performed by providing the above-mentioned selection function.

The sample liquid introducing portion 21g is hermetically closed by a cap 22. When introducing a sample liquid into the chamber 2, the cap 22 is removed and the sample liquid is injected into a microsyringe or the like.

To explain the operation of the chamber configured in this way, the carrier gas introduced from the carrier gas introduction section 24 of the Nepurizer N is discharged from the discharge hole 26, but at this time, the sample liquid 27 is transferred to the sample liquid suction section 25. It is sucked, turned into a mist, and discharged from the discharge hole 26. The atomized sample liquid 2 of an appropriate size is produced by the selective action of the atomized material contained in the chamber 2.
7 is introduced into the torch port 23 by carrier gas, and the atomized sample liquid 27 having other sizes adheres to the inner surface of the chamber 2 from the discharge hole 26 and flows down in the form of droplets or becomes larger. The atomized sample liquid 27 that passes by falls as it is and is combined with the sample liquid 27 accumulated on the bottom surface of the chamber 2. The combined sample liquid 27 is sucked by the carrier gas from the multi-sample liquid suction section 25, becomes a mist again, and is discharged from the discharge hole 26, and this circulation operation continues.

All of the sample liquid 28 in the thus sealed chamber 21 can be used for analysis. and,
As long as carrier gas is being introduced, chamber 2
Even if the sample liquid 27 in the torch is completely consumed, the plasma will not be extinguished because the carrier gas is introduced into the torch without inhaling air.

In the above-mentioned embodiments, the shape of the chamber is spherical, but it is not limited to a spherical shape, and may be an eggplant shape,
Any shape such as an ellipse is acceptable, and any shape that allows the atomized sample liquid discharged from the discharge hole of the nebulizer to adhere to the inner surface of the chamber and flow down as droplets along the inner surface is applicable. can do.

In addition, the chamber can be constructed in a split type so that the nebulizer 1 can be replaced, and furthermore, a cleaning port and a drying gas introduction port can be provided for the purpose of saving time in cleaning the chamber.

(f) Effects As explained above, according to the present invention, a closed circulation chamber is constructed which is equipped with a torch port and a sample liquid introduction part, and a nebulizer is provided inside the chamber, and the shape of the chamber is formed on the inner surface of the chamber. By creating a shape in which the attached atomized sample liquid flows down in the form of droplets, and by placing the torch port at a position offset from the discharge hole of the nebulizer, all of the sample liquid in the chamber can be analyzed. Since it can be used for multiple applications, there is no wastage of sample liquid, and it is possible to analyze extremely small amounts.Also, even if the sample liquid in the chamber runs out, air is not sucked in, so the plasma is not extinguished. Since there is no need for extra accessory devices such as inner pipes, sub-tanks, and tubes, the number of parts can be reduced and costs can be reduced.

[Brief explanation of drawings]

Figure 1 is a cross-sectional view of a conventional ICP emission spectrometer;
The figure is a sectional view of an embodiment of a closed circulation chamber for ICP analysis of the present invention. In the figure, 21 is a spherical chamber, 21a is a sample liquid introduction part, 22 is a cap, 23 is a torch port, N is a nebulizer, 24 is a carrier gas introduction part, 25 is a sample liquid suction part, 26 is a discharge hole, 27 indicates the sample liquid.

Claims (1)

[Claims] (1) A chamber having a shape that allows droplets of sample liquid adhering to the inner surface to flow down and comprising a torch port and a sample liquid introduction part, and a chamber provided within the chamber and protruding outside the chamber. A nebulizer comprising a carrier gas introduction part, a sample liquid suction part, and a discharge part; and a hermetic seal for ICP analysis, characterized in that the torch port is provided at a position offset from the discharge part of the nebulizer. Circulating chamber.