JPH02110351A - Introducing and monitoring method of sample in i.c.p emission spectral analyzing device - Google Patents

Abstract

PURPOSE:To realize highly accurate analysis irrespective of the viscosity of a sample by introducing said nebulized sample in a chamber to a condensing core measuring device, monitoring the number of nebulized drops by said condensing core measuring device and adjusting the flow of a carrier gas to a nebulizer by a gas control unit. CONSTITUTION:In a high frequency induction coupling plasma (I.C.P) emission spectral analyzer for analyzing elements composing a sample which emits light in plasma of an inert gas such as argon gas, a condensing core measuring device 20 is connected to a supply port 16c of a chamber 16. The measuring device 20 counts the number of nebulized drops of a nebulized sample and feeds the counting value to a gas control unit 12 as a signal S20. For example, a nebulized drop having a particle size not smaller than 0.05mum is made to grow by diethylene glycol and, the number of the drops is counted by a laser diffusion light. Accordingly, the introducing amount of the nebulized sample to a torch 17 can be made constant.

Description

DETAILED DESCRIPTION OF THE INVENTION (Industrial Application Field) The present invention provides I, C, P for analyzing sample constituent elements that emit light in plasma of an inert gas such as argon gas.
, (Inductively Coupled Pl
The present invention relates to a method for monitoring sample introduction in an optical emission spectrometer (asma, high frequency inductively coupled plasma).

(Prior art) Conventionally, this type of 1. As a C, P, emission spectrometer, for example, the brand name rSEIKOJ, 5PS120O is used.
There is a type A device, whose configuration is shown in FIG.

This 1. The C, P, emission spectrometer is equipped with a gas control section 2 that introduces a carry gas 1 made of argon gas and supplies a flow-controlled carry gas GI, plasma gas G2, auxiliary gas 03, and the like. A carrier gas G1 is supplied to a nebulizer 3, and a liquid sample 4 is supplied to the nebulizer 3 through a capillary tube 5. A chamber 6 having a drain port 6a and a supply port 6b is connected to the ejection port side of the nebulizer 3, and a torch 7 is connected to the supply port 6b. The torch 7 has an introduction lower a for plasma gas G2 and an introduction lower b for auxiliary gas G3. A coil 8 is attached to the outer periphery of the torch 7, and the coil 8 is connected to a high frequency power source 9.

In the above configuration, the sample 4 introduced into the plasma flame F is supplied to the nebulizer 3 through the thin tube 5. The sample 4 supplied to the nebulizer 3 is supplied with carrier gas G1
The water is blown into the chamber 6 in the form of a mist. Among the atomized samples in the chamber 6, large-sized mist droplets are discharged as a train from the drain port 6a, and only small-sized mist droplets are passed through the supply port 6b to the plasma flame F of the torch 7.
will be introduced into the. The atomized sample introduced into the plasma flame F is excited by the energy of the plasma flame F and emits light by itself. Since each element in the sample 4 has a unique emission spectrum, by analyzing the emission spectrum with a spectrometer, the type of element in the sample 4 and its content can be measured.

This 1. C, P, in the emission spectrometer, nebulizer 3
The liquid sample 4 is atomized using the same principle as "fogging",
Introduced into plasma flame F.

The nebulizer 3 uses high frequency inductively coupled plasma (I).

C, P,) is the key to analysis, and generating a fine and uniform fog is necessary for measurement accuracy and stability. If the state of fog generation changes, the amount of atomized sample introduced into the plasma flame F will change, causing the measured value to fluctuate. Therefore, the gas control unit 2 adjusts the pressure of the carrier gas G1 based on a preset value to maintain the amount of mist generated at a constant value.

Therefore, in a sample analysis method using this type of device, the elements to be analyzed can be freely selected, the high-sensitivity analysis line and the low-intensity analysis line can be used freely, which saves the effort of diluting the sample 4, and the spectrometer It has the advantage that high-precision analysis is possible through the use of .

(Problem to be Solved by the Invention) However, in the sample analysis method using the device with the above configuration, the amount of the atomized sample introduced into the torch 7 is monitored (monitored).
Therefore, when the sample 4 is atomized with the nebulizer 3, the particle size of the atomized droplets varies depending on the viscosity of the sample 4, and the amount of atomized sample introduced into the plasma flame F changes. do. Therefore, there is a problem that a difference occurs in the amount of emission spectrum and accurate analysis cannot be performed, and it has been difficult to solve this problem.

The present invention solves the problem that the prior art had in that the viscosity of the liquid sample causes a difference in the amount of emission spectrum, reducing analysis accuracy. This provides a monitoring method.

(Means for Solving the Problems) In order to solve the above problems, the present invention provides an I, C, P, emission spectrometer equipped with a gas control section, a nebulizer, a chamber, a torch, and a spectrometer. A condensation nucleus measuring device that counts the number of condensation nuclei is connected to the chamber, the number of atomized droplets of the atomized sample supplied from the chamber is counted by the condensation nucleus measuring device, and the condensation nuclei are supplied from the gas control section according to the counted value. The flow rate of the carrier gas is adjusted.

(Function) According to the present invention, the spray state of the sample is monitored by counting the number of mist droplets using a condensation nucleus measuring device. Feedback of the monitoring results to the gas control section allows the gas control section to adjust the amount of carrier gas supplied, making the amount of atomized sample introduced into the torch constant regardless of the viscosity of the sample. There is work. Therefore, the above problem can be solved.

(Example) FIG. 1 is a diagram illustrating a detailed explanation of the present invention.

FIG. 3 is a configuration diagram of a c,p, emission spectrometer.

This r, c, p, emission spectrometer has a gas control unit 12 that adjusts the flow rate of a carrier gas 11 made of an inert gas such as argon gas to be supplied to the plasma.
have. This gas control section 12 has a signal S
It has a function of adjusting the flow rate and pressure of carrier gas Gll based on 20, and also has a function of adjusting plasma gas G12 and auxiliary gas 013. A carrier gas Gll is supplied to the nebulizer 13, and a sample 14 of liquid such as sulfuric acid (HSo), phosphoric acid (H3P04), etc. is supplied to the nebulizer 13 through a capillary tube 15. The nebulizer 13 atomizes the liquid sample 14 using the negative pressure caused by the high-speed flow of the carrier gas G11 based on the same principle as "atomizing", and its ejection port side is connected to the chamber 16.
It is connected to the.

The chamber 16 has a function as a buffer for efficiently sending the atomized sample to the plasma flame F, and has a drain port 16.
a, and supply ports 16b and 16c. Supply port 1
A torch 17 is connected to 6b. Torch 17 is
Inlet port 17a for plasma gas G12 and auxiliary gas 013,
17b, generates plasma with plasma gas G12, floats the plasma with auxiliary gas 013,
It has the function of introducing the atomized sample from the chamber 16 into the center of the plasma. A coil 18 for generating a magnetic field is attached to the outer periphery of the torch 17, and the coil 18 is connected to a high frequency power source 19.

Further, a condensation nucleus measuring device 20 is connected to the supply port 16c of the chamber 16. The condensation nucleus measuring device 20 is a device that counts the number of mist droplets of an atomized sample and supplies the counted value to the gas control unit 12 in the form of a signal S20. The structure is such that the mist droplets themselves grow and the number of mist droplets is counted using laser scattered light.

Next, 1. of the above configuration. A method for monitoring sample introduction using a C, P, and emission spectrometer will be explained.

The carrier gas Gll is supplied from the gas control unit 12 to the nebulizer 13, and the plasma gas G1
When the auxiliary gas G13 and the auxiliary gas G13 are supplied to the torch 17, the nebulizer 13 sucks the liquid sample 14 through the thin tube 15 using the carrier gas Gll, atomizes the sample 14, and injects the sample 14 into the chamber 16. Among the atomized samples blown into the chamber 16, the mist droplets with relatively large particle sizes adhere to the inner wall of the chamber 16 and flow out as water droplets, that is, drains, toward the drain nozzle 16a. The mist droplets are supplied from the supply port 16b.

It is supplied to the torch 17 and condensation nucleus measuring device 20 side through 16c.

In the torch 17, high-frequency power supplied from the high-frequency power supply 19 causes a high-frequency current to flow through the coil 18 and generate a magnetic field, so plasma is generated by the plasma gas G12 introduced from the introduction port 17a, and plasma is introduced from the introduction port 17b. The auxiliary gas 013 causes the internal plasma to float up and become a plasma flame F. And chamber 16
The atomized sample entering the torch 17 from the supply port 16b is introduced into the plasma flame F. The metal element contained in the sample 14 introduced into the plasma flame F receives the energy of the plasma flame F, changes from a ground state to an excited state, and emits light with a unique emission spectrum. Since this emission spectrum differs for each element, by analyzing these emission spectra with a spectrometer (not shown), the types and amounts of elements contained in the sample 14 can be measured.

Here, the condensation nucleus measuring device 20 measures the atomized sample supplied from the supply port 16c of the chamber 16, for example, with a particle size of 0.
Count the number of mist droplets larger than 0.05μ.

Mist droplets from highly viscous samples (e.g., H2SO4, H3PO2, etc.) have large particle sizes, resulting in low counts; however, mist droplets from low-viscosity samples have very small particle sizes, making it difficult to count. The number increases.

When these count values are sent to the gas control unit 12 in the form of a signal S20, the gas control unit 12 outputs a signal S2.
0, the flow rate and pressure of the carrier gas Gll supplied to the nebulizer 13 are adjusted so that the count value in the condensation nucleus measuring device 20 is a constant value, that is, the count value is a constant value for the sample and the standard solution. Control as shown. Therefore, the number of droplets of the atomized sample introduced into the plasma flame F is constant, and the analysis value does not fluctuate due to the viscosity of the sample 14, making it possible to perform highly accurate analysis.

Note that the present invention is not limited to the illustrated embodiment; for example, the shape and structure of the chamber 16, or the supply ports 16b, 16c
■ by changing the formation position, etc.

The performance of the device may be improved by changing the components of the c,p, emission spectrometer into other shapes and structures, or by adding other elements.

(Effects of the Invention) As described in detail above, according to the present invention, an atomized sample in a chamber is introduced into a condensation nucleus measuring device, the number of atomized droplets is monitored by the condensation nucleus measuring device, and gas control is performed. Since the flow 1 of the carrier gas to the nebulizer is adjusted depending on the chamber, the number of mist droplets in the chamber can be maintained at a constant value, and the number of mist droplets introduced into the plasma is therefore constant. Highly accurate analysis can be performed regardless of the viscosity of the material.

[Brief explanation of the drawing]

FIG. 1 is a diagram (■) for detailed explanation of the present invention. c, p, Configuration diagram of the emission spectrometer, Figure 2 is the conventional 1
．． C, P, is a configuration diagram of an emission spectrometer. 11...Carrier gas, 12...Gas control section, 13...Nebulizer, 14
...Sample, 16...Chamber, 16a
...Drain port, 16b, 16c...
Supply port, 17... Torch, 18... Coil, 19... High frequency power supply, 20...
Condensation nucleus measuring device, F... Plasma flame, Gll.
...Carrier gas, G12...Plasma gas.

Claims (1)

[Scope of Claims] A gas control section that adjusts the supply amount of carrier gas and plasma gas, a nebulizer that atomizes a liquid sample with the carrier gas supplied from the gas control section, and atomization ejected from the nebulizer. a chamber for removing atomized droplets having a larger particle size than that in the sample; generating a magnetic field to generate plasma from the plasma gas supplied from the gas control section; and introducing the atomized sample supplied from the chamber into the plasma. I, which is equipped with a torch for introducing the plasma, and a spectrometer for separating the light of the elements in the sample generated in the plasma and selectively extracting only the light of the target element.
, C, P, in the emission spectrometer, a condensation nucleus measuring device for counting the number of mist droplets is connected to the chamber, and the number of mist droplets of the atomized sample supplied from the chamber is counted by the condensation nucleus measuring device. A method for monitoring sample introduction in an I, C, P, emission spectrometer, characterized in that the flow rate of a carrier gas supplied from the gas control section is adjusted according to the counted value.