JPH06249781A - Icp emission spectroscopic analyzer - Google Patents

Abstract

PURPOSE:To perform a measurement quickly by a method wherein, before a solution sample is atomized and measured, a spray chamber is adjusted to a prescribed temperature and the luminous intensity of a plasma torch is stabilized. CONSTITUTION:A timer 12 for a temperature controller 10 is operated before the prescribed time of a measuring operation on every operating day, and switches 16, 17 are closed. A detection signal by a temperature sensor 7 and a set signal by a temperature setter 11 are compared by a comparator 13, a heater 8 is driven by its output via a heater drive circuit 14, and, at the same time, a pump drive circuit 15 drives a pump 9. Thereby, water inside a storage tank is heated, it is introduced into a circulation chamber anti it heats a spray chamber. A measuring operator drives an analyzer, and a plasma torch is turned on and driven. When a carrier gas is introduced into the spray chamber, the temperature of the spray chamber is set to a temperature similar to that after a sufficient warm-up operation. Consequently, the luminous intensity of the plasma torch is not fluctuated, and the measuring operation can be started quickly.

Description

Detailed Description of the Invention

[0001]

The present invention relates to a high frequency inductively coupled plasma as a light source for emission spectroscopy.
The present invention relates to an ICP emission spectroscopic analyzer equipped with a plasma torch for generating an adio frequency plasma (ICP), and in particular, a nebulizer for atomizing the solution sample since the sample to be spectroscopically analyzed is a solution in this kind of device. And an atomization chamber for introducing the atomized sample into a plasma torch.

[0002]

2. Description of the Related Art FIG. 3 is a schematic configuration diagram of a conventional ICP emission spectroscopic analysis device of this type. In this device, a nebulizer 1 or a plasma torch 2 is a plasma emission chamber surrounded by a housing 3. While equipped inside,
The solution sample S is supplied from the outside of the housing 3. Coolant gas for cooling and plasma gas for combustion are introduced from the outside into the plasma torch 2 having a triple structure of quartz tube, while the solution sample S is atomized by the nebulizer 1. After being introduced into the spray chamber 1a together with the carrier gas for homogenizing the sample, the plasma is guided to the plasma torch 2 and excited by the plasma generated by being driven by the high frequency electric power for emission spectroscopic analysis. Then, this emitted light is guided to a spectroscopic analysis chamber 5 adjacent to the plasma emission chamber through a window 4 provided in the housing 3, and contained in the sample by a spectroscopic analyzer (not shown) in the spectroscopic analysis chamber 5. Spectral lines that are peculiar to the element
The presence and intensity of each spectral line is detected, and the qualitative and quantitative analysis of each element contained in the sample is performed.

[0003]

By the way, the above-mentioned I
In the CP emission spectroscopic analyzer, the emission intensity of the plasma torch 2 fluctuates immediately after the start of the spectroscopic analysis of the sample, and therefore the measured value of the sample is not stable, so that there is no variation in the emission intensity and stable measurement is performed. It is known that the apparatus itself must be warmed up (warm-up) for a predetermined period of time, for example, 30 minutes to 1 hour in advance, before the operation is started.

However, if there is such a long warm-up operation before the actual measurement, the actual time in which the device itself can be used for the measurement is shortened and the efficiency in use thereof is lowered. There is also a problem that the carrier gas is consumed even during the warm-up operation, and the high frequency power for driving the plasma torch is wasted.

Therefore, the inventors of the present invention have examined the circumstances requiring the warm-up operation as described above, and found that the temperature of the spray chamber 1a of the nebulizer 1 is as low as room temperature at the start of the operation. , While continuing the operation,
After the temperature is raised by the heat generated by the plasma torch 2 and the like, the temperature is stabilized at a certain temperature higher than room temperature by a predetermined temperature, and in the process of such temperature rise, the atomized state of the sample in the spray chamber 1a of the nebulizer 1 is successively increased. It was found that the emission intensity of the plasma torch 2 fluctuates in order to change.

An object of the present invention is to solve the conventional problems in accordance with the above-mentioned findings and to enable actual measurement of a sample early after the start of operation.

[0007]

According to the present invention, in order to achieve the above object, a solution sample is jetted into a spray chamber by a nebulizer, atomized, and then introduced into a plasma torch.
The CP emission spectroscopic analyzer is characterized in that it is provided with temperature adjusting means for adjusting the spray chamber to a predetermined temperature before required measurement of the solution sample by the device.

[0008]

According to the above construction, the temperature of the spray chamber in which the liquid sample is atomized can be warmed by the temperature adjusting means as if immediately after the warm-up operation, so that the plasma torch can be used. The emission intensity of is stable, and the measurement will be started early after the start of operation.

[0009]

DESCRIPTION OF THE PREFERRED EMBODIMENTS FIG. 1 is a block diagram showing a schematic structure of an ICP emission spectroscopic analyzer according to an embodiment of the present invention, and FIG. 2 is a circuit block diagram of a main part of FIG. Portions similar to or corresponding to those in FIG. 3 according to the example are denoted by the same reference numerals, and detailed description of the portions having the same reference numerals is omitted.

As will be described with reference to FIG. 1, in the IPC emission spectroscopic analyzer of the present embodiment, the outer periphery of the spray chamber 1a of the nebulizer 1 is covered with a heated water circulation chamber 1b, and its heating is performed. The water circulation chamber 1b is provided with a heating water inlet 1c and a heating water outlet 1d. The heating water introduced from the heating water inlet 1c passes through the outer periphery of the spray chamber 1a and then from the heating water outlet 1d. A temperature adjusting means 6 is provided for adjusting the temperature of the spray chamber 1a by adjusting the temperature of the heating water that is to be discharged and that passes through the outer periphery of the spray chamber 1a.

The temperature adjusting means 6 is provided around the outer periphery of the spray chamber 1a and detects the ambient temperature of the spray chamber 1a, and a storage tank 18 for storing water to be supplied to the circulation chamber 1b. A heater 8 provided inside the storage tank 18 for heating the water in the storage tank 18 to generate heated water; and a pump 9 for circulating the water in the storage tank 18 in the heated water circulation chamber 1b.
And a temperature controller 10 for controlling the temperature of the heated water.

The temperature controller 10 includes a heater 8 in response to a temperature detection signal of the heated water detected by the temperature sensor 7.
Also, it controls the operation of the pump 9, and the temperature setter 11 and the timer 12 are connected for controlling the operation. The timer 12 is set to the start time of the device, and when the measurement operator of the device, for example, a measurement operator uses the device to measure the sample, the temperature adjusting means 6 can immediately perform the measurement. The temperature controller 10 drives the heater 8 and the pump 9 in response to the activation signal to activate the heater 8 and the pump 9 in order to activate the circulation chamber 1b. The spray chamber 1a is heated by supplying heated water therein. The temperature setter 11 inputs data for setting the temperature of the spray chamber 1a to a predetermined temperature, and the measurement operator operates the temperature setter 11 to instruct the temperature controller 10 of the spray chamber 1a. It gives a setting signal for setting the temperature. In response to the input of the timer 12, the temperature controller 10 drives the heater 8 so as to control the temperature of the spray chamber 1a to the temperature corresponding to the setting signal.

The temperature controller 10 will be described in detail with reference to FIG. First, structurally, the temperature controller 10 drives a heater 8 according to a comparison output of the comparator 13 that compares a setting signal from the temperature setting device 11 with a detection signal from the temperature sensor 7, and a comparison output of the comparator 13. A heater drive circuit 14 for driving the pump 9, a pump drive circuit 15 for driving the pump 9, a switch 16 provided on the output side of each drive circuit 14, 15 and closed in response to the output of the timer 12.
17 and 17.

In the temperature controller 10 having the above-described structure, the timer 12 measures the sample at a predetermined time of each work day, for example, when a measurement worker comes to the place where the device is installed and operates the device. The switches 16 and 17 are closed by operating a predetermined time before performing work. Then, the heater drive circuit 14 drives the heater 8 by the output of the comparator 13 of the detection signal from the temperature sensor 7 and the setting signal from the temperature setter 11, while the pump drive circuit 15 drives the pump 9. As a result, the heater 8 and the pump 9 are driven to heat the water in the storage tank 18, and the heated water is introduced into the circulation chamber 1b through the heated water inlet 1c of the circulation chamber 1b, and the spray chamber 1a is heated. Then, the circulating heated water in this case is controlled to a constant temperature by the temperature controller 10 and the temperature of the spray chamber 1a is maintained at a constant level. Therefore, the measurement operator drives the apparatus and the plasma torch with high frequency power. When 1 is driven to be driven and carrier gas is introduced into the spray chamber 1a,
The temperature of the spray chamber 1a has been warmed to the same state as immediately after the warm-up operation is sufficiently performed.
Therefore, at the time when the measurement operator uses the device to measure the sample, even if the nebulizer 1 atomizes the solution sample, it can be aerosolized in a constant atomized state, and the plasma torch 2 emits light with a high emission intensity. Since there is no fluctuation, the measurement operator can start the measurement operation immediately after turning on the plasma torch 2 without performing any warm-up operation.

In the above-mentioned embodiment, the temperature adjusting means 6 is automatically operated by the timer 12, but it goes without saying that the temperature adjusting means 6 may be operated by the operation of the measuring operator. In that case as well, the spray chamber 1a is forcibly warmed, so that the measurement work can be started early with a very short warm-up operation.

Further, as another embodiment of the present invention, in addition to the structure of the above-mentioned embodiment, means for adjusting the ambient temperature in the entire housing 3, for example, a heater and a fan are provided in the housing 3 to provide the housing 3 The ambient temperature inside may be adjusted.

When an organic solvent is used as the sample solvent, when the temperature of the spray chamber 1a rises, the organic solvent vaporizes and extinguishes the plasma. Therefore, as another embodiment of the present invention, In this case, the temperature of the spray chamber 1a may be adjusted to be low, that is, the spray chamber 1a may be cooled.

[0018]

According to the present invention, since the temperature of the spray chamber is adjusted by the temperature adjusting means, for example, by forcibly warming the temperature of the spray chamber, the fluctuation of the emission intensity in the plasma torch does not occur and the worm is warmed. The up operation can be omitted or rounded up in a short time, and the measurement work can be started early, and the device can be used efficiently.

Further, since the warm-up operation can be shortened or omitted, it is possible to save the carrier gas and the electric power which are conventionally consumed in the warm-up operation.

[Brief description of drawings]

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

FIG. 2 is a circuit block diagram of a temperature controller portion of the above embodiment.

FIG. 3 is a configuration diagram of a main part of a conventional ICP emission spectroscopy analyzer.

[Explanation of symbols]

 1 Nebulizer 2 Plasma torch 3 Housing 6 Temperature adjusting means 7 Temperature sensor 8 Heater 9 Pump 10 Temperature controller

Claims (1)

[Claims] 1. An IC in which a solution sample is jetted into a spray chamber by a nebulizer and atomized and then introduced into a plasma torch.
The P emission spectroscopic analyzer is provided with a temperature adjusting means for adjusting the spray chamber to a predetermined temperature before required measurement of the solution sample by the device.
Optical emission spectrometer.