JPH0656362B2 - Closed circulation chamber for ICP analysis - Google Patents

Description

Detailed Description of the Invention (a). BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a closed circulation type chimba for introducing a liquid sample, which is used for emission spectroscopic analysis using ICP (high frequency induction plasma).

(B). In the conventional emission spectroscopic analysis using ICP as a light source, a high-frequency current with a frequency of 300 MHz or less is passed through a coil, and discharge is caused by electrolysis generated by electromagnetic induction due to the time change of the high-frequency magnetic field. A mist-like sample is introduced into the holes formed in the generated plasma to excite it, and the wavelength and intensity of the light emitted at that time are measured by a spectrometer to perform qualitative and quantitative analysis of the sample.

A conventional ICP emission spectroscopic analyzer of this type will be described with reference to FIG.

In the figure, 1 is a sample container, and the 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 made by the introduced carrier gas.
And a discharge port 6 for discharging the mist as a mist. 7 is a chimba made of Pyrex glass, and a torch port 7 integrally formed with this chimba 7.
a, a discharge portion 7b for the atomized sample liquid 2 not introduced into the torch port 7a, and a large-diameter opening portion 7c.
The opening 7c is airtightly closed by the holder 8, and the nebulizer N is fitted in the holder 8 while keeping the airtight state. Reference numeral 9 is an inner tube similarly made of pyrex glass, and is connected to the chain 7.
A tube 10 is connected to the discharge part 7b of the chain 7,
The other end of the tube 10 is connected to a pipe provided on the bottom surface of the sub tank 11, and the sub tank 11
And water is stored in the tube 10. This water is
For the purpose of introducing the carrier gas and the atomized liquid sample 2 introduced into the inner tube 9 through the discharge hole 6 into the torch port 7a, they are stored to prevent decompression of the chamber 7. 15 is a torch made of quartz, and the torch port 7
An induction coil 16 is wound around the torch 15 and is connected to a, and a plasma light source 17 is generated.

Explaining the operation of the device thus configured,
Due to the carrier gas introduced into the carrier gas introduction hole 5, the sample liquid 2 in the sample container 1 is introduced into the nebulizer N via the sample liquid introduction hole 4 via the tube 3, and is connected to the atomization body from the discharge hole 6 through the chimney. 7 is discharged to the inner pipe 9. Other than the atomized sample liquid 2 having a size suitable for being introduced into the torch 15 through the torch port 7a, the sample liquid 2 drops into the inner tube 9 or adheres to the inner surface thereof, or the chimney 7
Adheres to the inner wall of the container, flows down as drops, and is united with the water present in the discharge part 7b. From the sub-tank 11, the amount of the sample liquid 2 combined with water is discharged into the waste liquid container 13 through the tube 12, and the mixed liquid 1 of water and the sample liquid 1 is discharged.
4 is filled in the waste liquid container 13.

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 any other size is stored in the tube 10. Since it is combined with the water of the above and discarded to the outside, only about 5% of the sample liquid is actually used for the analysis, and about 95% of the other is wasted. In addition, since the amount of collected biological samples is extremely small, it is necessary to collect a large amount of biological samples in order to use it in an ICP emission spectroscopic analyzer.

Further, the sample liquid 2 in the sample container 1 is all nebulizer N
After the gas has been introduced into the chamber, air will be introduced, and this will cause the plasma to disappear, so the sample container 1 must always be kept empty during the analysis. It was

(C). The present invention solves the above-mentioned drawbacks of the prior art, in which a sample liquid for analysis is introduced into a chimba, which is made into a mist by a nebulizer, and the sample liquid dropped without reaching the torch is atomized again. It is an object of the present invention to provide a closed circulation type chimba for ICP analysis in which the whole circulation of the liquid is reversed and the whole sample liquid can be used for the analysis.

(D). Structure According to the present invention, the chimba has a closed structure, and the sample liquid in the chimba is made into a mist by a nebulizer, and this is introduced into the torch. All of the sample liquid can be consumed for the analysis by bringing the sample liquid into a single unit and circulating it to atomize it again.

(E). EXAMPLE An example of the closed circulation type chamber for ICP analysis of the present invention will be described with reference to FIG.

In the figure, 21 is a spherical closed type chamber made of pyrex glass, and is provided with a torch port 23 and a sample liquid introduction part 21a. A nebulizer N is provided in the chimney 21, and the nebulizer N is provided with a carrier gas introduction part 24, a sample liquid suction part 25, and a discharge hole 26 for discharging the atomized sample liquid. The carrier gas introduction part 24 is kept airtight and is projected to the outside through the chamber 21. Further, the nebulizer N is provided so as to be located at the center of the chamber 21, and also has a lower end surface of a sample liquid suction unit 25 for sucking the sample liquid 27 in the chamber 21,
The distance from the inner surface (bottom surface) of the chamber 21 facing this is set to be about 0.3 to 0.5 mm, and the discharge hole 26 connected to the sample liquid introduction part 25 is located above.

The torch port 23 is provided at a position deviated from the carrier gas discharge direction so as not to directly face the discharge direction of the carrier gas introduced from the carrier gas introduction part 24 from the discharge hole 26. The reason for such a positional relationship is that the atomized liquid sample 27 having various sizes discharged from the discharge hole 26 of the nebulizer N is directly fed to the torch port 23.
In order to prevent the analysis accuracy from being lowered by being introduced into the torch and analyzed through the torch, a nebulizer N discharge hole 26 and a discharge hole 26 of the nebulizer N can be selected so that an atomized sample liquid 27 of an appropriate size can be selected. This is for avoiding the facing position and for providing the offset position so that the selecting action described above is performed.

The sample liquid introducing portion 21a is hermetically closed by a cap 22, and when introducing the sample liquid into the chamber 21, the cap 22 is removed and the sample liquid is injected by a microcylinder or the like.

Explaining the operation of the chimba thus configured, the carrier gas introduced from the carrier gas introduction part 24 of the nebulizer N is discharged from the discharge hole 26. At this time, the sample liquid 27 is sucked into the sample liquid suction part 25. , And is discharged from the discharge hole 26 in the form of mist. The atomized sample liquid 2 having an appropriate size due to the selective action of the atomized body of the chimney 21
Only 7 is introduced into the torch port 23 by the carrier gas, and the atomized sample liquid 27 having other sizes is 26
The sample liquid 27 that adheres to the inner surface of the chamber 21 and flows down as a drop or is too large is dropped as it is, and is combined with the sample liquid 27 accumulated on the bottom surface of the chamber 21. The combined sample liquid 27 is sucked from the sample liquid suction portion 25 by the carrier gas, is again atomized and is discharged from the discharge hole 26, and such a circulating operation is continued.

The sample liquid 27 in the chamber 24 thus sealed can be used for analysis. And
As long as carrier gas is being introduced, Chiemba 2
Even if the sample liquid 27 in 1 is consumed, air is not sucked in and the carrier gas is introduced into the torch, so that plasma is not extinguished.

In the above-mentioned examples, the shape of chiemba was described as a spherical shape, but the shape is not limited to a spherical shape, and an eggplant type,
It may be oval or the like, and it is applicable as long as the atomized sample liquid discharged from the discharge hole of the nebulizer adheres to the inner surface of the chimba and can flow down as drops along the inner surface. can do.

Further, the chimney can be configured as a split type, the nebulizer can be replaced, and a cleaning port and a gas introduction port for drying can be provided for the purpose of saving time for cleaning the inside of the chimba.

(F). Effect As described above, according to the present invention, a closed circulation type chimba having a torch port and a sample liquid introduction part and having a nebulizer inside thereof is constituted, and the shape of the chimba is a fog attached to the inner surface thereof. -Shaped sample liquid flows down as drops, and by providing the torch port at a position offset from the discharge hole of the nebulizer, the entire sample liquid in the chimney can be used for analysis. Since there is no waste of the sample liquid, it is possible to analyze a very small amount, and even if the sample liquid in the chimba is exhausted, air is not sucked in, plasma is not extinguished, and the inner tube and sub-tank like the conventional device Since no extra accessories such as a cable and a tube are required, the number of parts can be reduced, the configuration can be simplified, and the cost can be reduced. .

[Brief description of drawings]

FIG. 1 is a cross-sectional view of a conventional ICP emission spectroscopic analyzer, and FIG. 2 is a cross-sectional view of an embodiment of a closed circulation type 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 is a A sample liquid is shown.

Claims (1)

[Claims] 1. A chimba having a shape capable of allowing a drop of a sample liquid adhering to the inner surface thereof to flow down, and having a torch port and a sample liquid introduction part; and a sample liquid suction part provided in the chimba. And a carrier gas introduction part projecting outside of the chamber, the sample liquid suction part being located close to the bottom surface of the chamber and the discharging part being located above. A nebulizer configured so that the carrier gas introduced from the discharge portion is discharged from the discharge portion, and the torch port is provided at a position that does not directly face the discharge direction of the carrier gas from the discharge portion. A closed circulation type chimba for ICP analysis.