JPH06249783A - Icp emission spectroscopic analyzer - Google Patents

Abstract

PURPOSE:To simultaneously analyze various kinds of chemical elements by a method wherein a hydride from a generator and an atomized sample from a nebulizer are introduced into two sample introduction tubes for a plasma torch. CONSTITUTION:An analyzer 1 is provided with two sample introduction systems for a hydride generator 2 and an ultrasonic nebulizer 3. The generator 2 is provided with a joint part 5 which introduces a liquid sample S, a hydrogenating agent and a carrier gas, with a coil-shaped reaction tube 6 and with a gas-liquid separation chamber 8 which is connected to it via a communication tube 7. The nebulizer 3 is provided with a nebulizer main body 13 which atomizes the sample by ultrasonic vibrations and with a solvent-removing part 14. A plasma torch 21 is provided with two sample introduction tubes so that a hydride from the generator 2 and an atomized sample from the nebulizer 3 can be introduced together with a coolant gas and a plasma gas. Thereby, chemical elements such as As, Se, Sb and the like which fall short of a sensitivity by the nebulizer 3 only as well as Cd, Fe, Zn and the like which cannot be changed into a gas hydride can be analyzed simultaneously, and the analytical efficiency of the title analyzer can be enhanced.

Description

Detailed Description of the Invention

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to an ICP (high frequency inductively coupled plasma) emission spectroscopic analyzer, and more particularly to improvement of a sample introduction system thereof.

[0002]

2. Description of the Related Art Generally, a sample introduction system of an ICP emission spectral analyzer is shown in FIGS.

First, in the sample introduction system shown in FIG. 3, the liquid sample S in the sample container 18 is jetted toward the inside of the spray chamber 27 by the nebulizer 25 of the spraying type and atomized, and the atomized sample is transferred to the carrier pipe 28. It is introduced into a plasma torch 30 having a triple tube structure via a high frequency coil 22, and the high frequency magnetic field generated by the high frequency coil 22 excites and emits the atomized sample for analysis.

Further, the sample introduction system shown in FIG. 4 is an ultrasonic nebulizer 3 capable of obtaining a sample aerosol having a finer particle size than that of the above-mentioned nebulizer 25 of the atomizing system.
Is an introduction system using. The ultrasonic nebulizer 3 is composed of a nebulizer body 13 that atomizes the liquid sample S by ultrasonic vibration and a desolvation unit 14, and a spray chamber 15
The liquid sample S supplied via the pump 19 to the ultrasonic vibrator 16 therein is atomized by the vibration of the ultrasonic vibrator 16 and sent to the desolvation unit 14 together with the carrier gas. While heating and drying in the heating stage 14a of
The solvent is removed by cooling in the cooling stage 14b and then introduced into the plasma torch 30.

Further, the sample introduction system shown in FIG. 5 is an introduction system having a hydride generator 2 which reduces the elements in the liquid sample S to convert them into gaseous hydrides and then introduces them into the plasma torch 30. is there.

When both the liquid sample S, the hydrogenating agent and the carrier gas are introduced into the joint portion 5 of the hydride generator 2, most of the liquid sample S reacts with the hydrogenating agent when passing through the reaction tube 6. As a result, hydride is produced, and a part of the unreacted hydrogenating agent and the liquid sample are directly introduced into the gas-liquid separation chamber 8. The gas-liquid separation chamber 8 is for separating the hydride M obtained in the reaction tube 6 from the reaction residual liquid L and stabilizing the analysis sensitivity. Are sent to the plasma torch 30. At the lower part of the gas-liquid separation chamber 8, an S-shaped tube 9 for adjusting the liquid level and each end of a rapid discharge tube 10 for discharging the reaction residual liquid L at the time of exchanging the sample liquid are respectively connected, and the S-shaped tube is The other ends of 9 and the rapid discharge pipe 10 are both open to the drain tank 11.

[0007]

However, in the sample introduction system using the atomizing nebulizer 25 shown in FIG. 3 or the ultrasonic nebulizer 3 shown in FIG. 4, As,
Elements such as Se, Sb, and Bi cannot be analyzed due to insufficient sensitivity. Therefore, in the analysis of such elements, the elements are reduced by the sample introduction system using the hydride generator 2 shown in FIG. It is necessary to convert it into a gas hydride for analysis. On the contrary, since elements such as Cd, Fe, Zn, and Cr cannot be converted into a gas hydride, the nebulizer 25 or the ultrasonic nebulizer 3 of the atomization method is used. It needs to be analyzed using a sample introduction system.

Therefore, in the conventional ICP emission spectroscopic analyzer, when analyzing a sample containing both the elements such as As, Se, Sb and Bi and the elements such as Cd, Fe, Zn and Cr described above, It is necessary to replace the introduction system and perform the analysis twice. Therefore, the analysis is troublesome, and in the meantime, a large amount of argon gas is consumed and the analysis cost is high.

The present invention has been made in view of the above points, and it is an object of the present invention to enable simultaneous analysis of many kinds of elements without replacing the sample introduction system.

[0010]

In order to achieve the above-mentioned object, the present invention provides a hydride generator for reducing elements in a liquid sample to convert them into hydrides, and a nebulizer for atomizing the liquid sample. And a plasma torch having at least two sample introduction tubes, wherein the hydride from the hydride generator and the nebulizer atomized sample are individually introduced into each sample introduction tube of the plasma torch. I am trying.

[0011]

According to the above construction, the hydride from the hydride generator and the nebulizer atomized sample are simultaneously introduced into the plasma torch having a quadruple tube structure having two sample introduction tubes. It is possible to simultaneously analyze elements such as As, Se, Sb, and Bi, which lack sensitivity in the sample introduction system, and elements such as Cd, Fe, Zn, and Cr, which cannot be converted into gas hydrides.

[0012]

Embodiments of the present invention will now be described in detail with reference to the drawings.

FIG. 1 is a block diagram showing the entire ICP emission spectroscopic analyzer according to an embodiment of the present invention. The parts corresponding to the above-mentioned conventional example are designated by the same reference numerals.

ICP emission spectroscopic analyzer 1 of this embodiment
Is equipped with two sample introduction systems, a hydride generator 2 and an ultrasonic nebulizer 3.

The hydride generator 2 has a structure similar to that of the conventional example shown in FIG. 5, and a joint portion into which a liquid sample S, a hydrogenating agent such as NaBH ₄ and a carrier gas such as Ar are introduced together. 5, a coil-shaped reaction tube 6 extending from the joint portion 5, and a gas-liquid separation chamber 8 connected to the reaction tube 6 via a communication tube 7.

The gas-liquid separation chamber 8 is for separating the hydride M produced in the reaction tube 5 from the reaction residue L and for stabilizing the analysis sensitivity. The S-shaped tube 9 for level adjustment and each one end of a rapid discharge tube 10 for discharging the reaction residual liquid L when exchanging the sample solution are connected to each other, and the other ends of the S-shaped tube 9 and the rapid discharge tube 10 are connected to each other. Also opens to the drain tank 11. A peristaltic pump 12 for forcibly discharging the reaction residual liquid L is provided in the middle of the rapid discharge pipe 10.

On the other hand, the ultrasonic nebulizer 3 has the same structure as that of the conventional example shown in FIG. 4, and comprises a nebulizer main body 13 for atomizing the liquid sample S by ultrasonic vibration and a desolvent section 14.

The nebulizer body 13 is provided with an ultrasonic vibrator 16 in the spray chamber 15. The carrier gas is sent into the spray chamber 15 through a carrier gas inlet pipe 17, and the ultrasonic vibrator 16 is also provided. The same liquid sample S as the sample sent to the hydride generator 2 from the sample container 18 by the drive of the pump 19 is sent to the surface of the liquid sample S, and the liquid sample S is fogged by the vibration of the ultrasonic transducer 16. And the sample aerosol is sent to the desolvation section 14 together with the carrier gas.

The desolvation section 14 includes a heating stage 14a at the front stage,
In the heating stage 14a, the sample aerosol from the nebulizer main body 13 is heated and dried to be fine particles, and in the cooling stage 14b, the vaporized solvent is condensed and removed from the sample aerosol by cooling.

The plasma torch 21 of this embodiment is arranged coaxially with the high frequency coil 22, and unlike the plasma torch 30 of the conventional triple tube structure, the hydrogen from the hydride generator 2 is supplied together with the coolant gas and the plasma gas. And a sample aerosol from the ultrasonic nebulizer 3 have a quadruple tube structure having two sample introduction tubes so that they can be introduced together.

In the ICP emission spectroscopic analyzer 1 having the above structure, when the liquid sample S, the hydrogenating agent, and the carrier gas are introduced into the joint portion 5 of the hydride generator 2 together, when passing through the reaction tube 6. Most of the liquid sample S and the hydrogenating agent react with each other to form a hydride, and a part of the unreacted hydrogenating agent and the liquid sample are introduced into the gas-liquid separation chamber 8 as they are. In the gas-liquid separation chamber 8, the unreacted liquid sample S and the hydrogenating agent are completely reacted here to generate a hydride M, and the gas hydride is a plasma torch 21 having a quadruple tube structure.
Is sent toward one of the sample introduction tubes.

On the other hand, in the ultrasonic nebulizer 3, the liquid sample S sent from the sample container 18 is sprayed and atomized by the ultrasonic vibrator 16 in the spray chamber 15, and the desolvation unit 14
Of the plasma torch 21 of the quadruple tube is heated and dried in the heating stage 14a of FIG. 1 to be finely granulated, and further cooled in the cooling stage 14b to remove the solvent from the sample aerosol. It is sent to the introduction pipe.

As a result, the plasma torch 21 has
Hydride from hydride generator 2 and ultrasonic nebulizer 3
The sample aerosol from the sample is introduced at the same time, excited and emitted, and analyzed.

As described above, since the hydride from the hydride generator 2 and the sample aerosol from the ultrasonic nebulizer 3 are simultaneously introduced into the plasma torch 21 for analysis, the sample introduction system using the nebulizer is insufficient in sensitivity. , S
Simultaneous analysis of elements such as e, Sb, and Bi and elements such as Cd, Fe, Zn, and Cr that cannot be converted into gaseous hydrides is possible. As in the conventional example, the sample introduction system is replaced and analysis is performed twice. It is not necessary, the analysis efficiency is improved, and the analysis cost can be reduced.

As described above, since it is possible to simultaneously analyze the elements such as As, Se, Sb, and Bi and the elements such as Cd, Fe, Zn, and Cr, the ICP emission spectroscopic analyzer 1 of the present invention is, for example, It is suitable for testing tap water.

FIG. 2 is a block diagram showing the entire ICP emission spectroscopic analyzer 1 ₁ of another embodiment of the present invention. The parts corresponding to those in the above embodiment are designated by the same reference numerals.

In this embodiment, the ultrasonic nebulizer 3 of the above-mentioned embodiment is replaced with a nebulizer 25 of a spraying type. This ICP emission spectroscopic analyzer 1 ₁ has a hydride generator 2 and a sprayer. Method nebulizer 25-2
Equipped with two sample introduction systems.

The nebulizer 25 of the atomization system has a nebulizer body 26 for atomizing a liquid sample S by jetting a carrier gas, and a nebulizer chamber 27 for homogenizing a sample aerosol obtained by atomizing the nebulizer body 26. The sample aerosol from the spray chamber 27 is
It is adapted to be introduced into one of the sample introduction pipes of the plasma torch 21 having a quadruple pipe structure via 8.

The other structure is the same as that of the above-mentioned embodiment.

Also in this embodiment, the hydride generator 2 is used.
And the sample aerosol from the atomizer 25 nebulizer 25 are simultaneously introduced into the plasma torch 21 having a quadruple tube structure, excited and emitted for analysis.

[0031]

As described above, according to the present invention, the hydride from the hydride generator and the sample atomized by the nebulizer are simultaneously applied to the plasma torch having the quadruple tube structure having at least two sample introduction tubes. As it is introduced, the sensitivity of As, Se, S is insufficient in the sample introduction system by the nebulizer.
Simultaneous analysis of elements such as b and Bi and elements such as Cd, Fe, Zn and Cr that cannot be converted into gaseous hydrides is possible, and it is necessary to replace the sample introduction system and analyze twice as in the conventional example. Therefore, the analysis efficiency can be improved and the analysis cost can be reduced.

[Brief description of drawings]

FIG. 1 is a configuration diagram of an ICP emission spectroscopy analyzer according to an embodiment of the present invention.

FIG. 2 is a configuration diagram of an ICP emission spectroscopy analyzer according to another embodiment of the present invention.

FIG. 3 is a configuration diagram of a conventional example including a nebulizer of a mist blowing system.

FIG. 4 is a configuration diagram of a conventional example including an ultrasonic nebulizer.

FIG. 5 is a configuration diagram of a conventional example including a hydride generator.

[Explanation of symbols]

1,1 ₁ ICP emission spectroscopy analyzer 2 hydride generator 3 ultrasonic nebulizer 21 plasma torch 25 nebulizer of atomization system

Claims (1)

[Claims] 1. A hydride generator for reducing an element in a liquid sample to convert it to a hydride, a nebulizer for atomizing the liquid sample, and a plasma torch having at least two sample introduction tubes, An ICP emission spectroscopic analyzer characterized in that the hydride from the hydride generator and the sample atomized by the nebulizer are individually introduced into each sample introduction tube of the plasma torch.