JPH10188877A - Inductively coupled plasma mass spectrometry device - Google Patents

Abstract

PROBLEM TO BE SOLVED: To perform sample switching in a short time and enable sample saving without leaving a previous analysis sample in a chamber by providing washing means for introducing a washing liquid in a spray chamber. SOLUTION: A liquid specimen 32 from a sample tank 31 and a carrier gas 34 via a gas flow rate control unit 33 are introduced into a nebulizer 35, and the liquid sample 32 is nebulized. A four-way cock 63 of washing means 60 is switched at one position, a carrier gas 34 and a same or different type of gas 52 are introduced into a spray chamber 36 via a blend gas line 51. When analysis of the sample 32 is completed, the four-way cock 63 of the washing means 60 is switched to another position to analyze a different specimen. A gas 52 is guided to a sealing tank 61, the washing water therein is introduced into the spray chamber 36, and the inside of the spray chamber 36 is washed.

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a nebulizer for introducing a sample of a carrier gas or a liquid and atomizing the sample, and introducing an atomized sample from the nebulizer.
The present invention relates to an inductively coupled plasma mass spectrometer comprising a spray chamber for condensing a mist having a large particle diameter in the atomized sample and discharging the condensate to the outside.

[0002]

2. Description of the Related Art Next, a conventional example will be described with reference to the drawings.
FIG. 3 is a configuration diagram of a conventional inductively coupled plasma mass spectrometer.

In FIG. 1, reference numeral 1 denotes a sample tank in which a liquid sample 2 is stored. 3 is a carrier gas (for example, Ar) 4
It is a gas flow control unit for controlling the flow rate of the gas. Reference numeral 5 denotes a nebulizer into which the carrier gas 4 from the gas flow controller 3 and the liquid sample 2 from the sample tank 1 are introduced, and the sample 2 is atomized.

A spray chamber 6 is attached to the nebulizer 5 via an adapter 7 and condenses mist having a large particle diameter in the atomized sample 2, and discharges the condensed liquid to the outside through the drain hole 6a.

[0005] 8 is a drain hole 6 of the spray chamber 6
This is a drain tank for storing the condensed liquid of the sample 2 discharged from a. Reference numeral 9 denotes an inductively coupled plasma (ICP) generated by a work coil 11 to which a sample atomized in a spray chamber 6 and a carrier gas 4 from a gas flow control unit 3 are introduced and a current is supplied from a high frequency power supply 10. 12
Is a plasma torch for ionizing the sample 2.

Reference numeral 13 denotes a mass spectrometer for obtaining the elements in the ionized sample 2 and the concentration of each element by utilizing the difference in the mass of the elements.

[0007]

However, when the sample 2 is analyzed in the inductively coupled plasma mass spectrometer having the above-described structure, the sample 2 'analyzed last time is sprayed by the spray chamber 6.
First, sample 2 'analyzed last time
The result of the analysis comes out (memory effect).

Therefore, there is a problem that the sample 2 must be continuously introduced into the nebulizer 5 until the previously analyzed sample 2 'remaining in the spray chamber 6 is completely replaced with the sample 2 to be analyzed this time. is there.

SUMMARY OF THE INVENTION The present invention has been made in view of the above problems, and an object of the present invention is to provide an inductively coupled plasma mass spectrometer capable of switching samples in a short time and saving samples.

[0010]

According to a first aspect of the present invention, there is provided a nebulizer for introducing a sample of a carrier gas or a liquid and atomizing the sample, and an atomized sample from the nebulizer. And an inductively coupled plasma mass spectrometer comprising a spray chamber for condensing a large particle size mist of the atomized sample and discharging the condensate to the outside, wherein a cleaning liquid is introduced into the spray chamber. An inductively coupled plasma mass spectrometer is provided with a cleaning means for performing the following.

After the sample analysis, a washing solution is introduced into the spray chamber by the washing means, and the remaining sample in the spray chamber is discharged outside the spray chamber. By washing away the residual sample in the spray chamber with the washing liquid, the next analysis does not require the introduction of the sample until the residual sample from the previous analysis is replaced, and the sample can be switched in a short time. In addition, the sample can be saved.

According to a second aspect of the present invention, there is provided the inductively coupled plasma mass spectrometer according to the first aspect of the present invention, wherein the cleaning means cleans an end of the spray chamber on the nebulizer side. .

By cleaning up to the end on the nebulizer side, sample switching can be performed in a very short time. The invention according to claim 3 is the invention according to claim 1 or 2, wherein the spray chamber is connected, and a blend gas line for introducing a gas of the same or different type as the carrier gas into the spray chamber is provided, and the cleaning is performed. A means is provided in the closed tank in which the cleaning liquid is stored, and in the blend gas line, when switching to one position, the gas flowing through the blend gas line is passed straight, and when switching to the other position, the blend gas line is switched. A switching means for guiding a flowing gas into the closed tank and sending a cleaning liquid in the closed tank to the blend gas line.

When the switching means is switched to one position, the same or different gas as the carrier gas flowing in the blend gas line is introduced into the spray chamber. When the switching means is switched to the other position, the same or different gas as the carrier gas flowing in the blend gas line is guided into the sealed tank, and the cleaning liquid in the sealed tank is introduced into the spray chamber via the blend gas line, The residual sample in the spray chamber is discharged out of the spray chamber.

By washing away the residual sample in the spray chamber with the cleaning liquid, it is not necessary to introduce the sample in the next analysis until the residual sample of the previous analysis is replaced, and the sample can be switched in a short time. And also saves on samples.

Further, the cost can be reduced by sharing the line for introducing the cleaning liquid into the spray chamber and the blend gas line. The invention according to claim 4 is
The cleaning solution according to any one of claims 1 to 3,
An inductively coupled plasma mass spectrometer characterized by being one of pure water and a water-soluble cleaning liquid.

By using one of pure water and a water-soluble cleaning liquid, switching can be performed more quickly than in the conventional method (replacement). As the water-soluble cleaning solution, there is a nitric acid aqueous solution.

[0018]

Embodiments of the present invention will now be described with reference to the drawings. (1) First Embodiment FIG. 1 is a configuration diagram of a first embodiment of the present invention. In the figure, reference numeral 31 denotes a sample tank in which a liquid sample 32 is stored. Reference numeral 33 denotes a gas flow controller that controls the flow rate of the carrier gas 34.

Reference numeral 35 denotes a nebulizer into which the carrier gas 34 from the gas flow controller 33 and the liquid sample 32 from the sample tank 31 are introduced, and the sample 32 is atomized. 3
Reference numeral 6 denotes a spray chamber which is attached to the nebulizer 35 via the adapter 37, condenses the mist having a large particle diameter among the atomized samples 32, and discharges the condensed liquid to the outside through the drain hole 36a.

Reference numeral 38 denotes a drain tank for storing the condensed liquid of the sample 32 discharged from the drain hole 36a of the spray chamber 36. Reference numeral 39 denotes an inductively coupled plasma (ICP) generated by a work coil 41 to which a sample atomized in a spray chamber 36 and a carrier gas 34 from a gas flow controller 33 are introduced, and a current is supplied from a high frequency power supply 40. 42 is a plasma torch for ionizing the sample 32.

Reference numeral 43 denotes a mass spectrometer for obtaining the elements in the ionized sample 32 and the concentration of each element by utilizing the difference in the mass of the elements. Reference numeral 51 denotes a blend gas line for introducing a gas (for example, nitrogen gas) 52 of the same or different type as the carrier gas 34 into the spray chamber 36.

The cleaning means 60 provided in the blend gas line 51 includes a closed tank 61 for storing a cleaning liquid 62 such as pure water or an aqueous nitric acid solution, and a cleaning tank 60 provided in the blend gas line 51. When the gas 52 flowing through the gas line 51 is passed straight through and switched to the other position, the gas 52 flowing through the blend gas line 51 is guided into the closed tank 61, and the cleaning liquid 62 in the closed tank 61 is passed through the blend gas line 51. It comprises a four-way cock 63 as a switching means for sending out to the spray chamber 36.

In this embodiment, the cleaning liquid is attached to the spray chamber 36 to attach the blend gas line 51.
And was provided so as to reach the end on the nebulizer 35 side. Next, the operation of the above configuration will be described. Nebulizer 3
5, a liquid sample 32 from a sample tank 31 and a carrier gas 34 are introduced via a gas flow controller 33, and the liquid sample 32 is atomized.

The atomized sample 32 is introduced into the spray chamber 36, and the mist having a large particle diameter among the atomized sample 32 is condensed and stored in the drain tank 38 through the drain hole 36a.

At this time, the four-way cock 63 of the cleaning means 60
Is switched to one position, and a gas 52 of the same or different type as the carrier gas 34 is introduced into the spray chamber 36 via the blend gas line 51.

The carrier gas 34 and the atomized sample 32
And a gas 52 of the same or different type as the carrier gas 34
The sample 32 is ionized by an inductively coupled plasma (ICP) 42 generated by a work coil 41 which is inserted into a plasma torch 39 and supplied with a current from a high frequency power supply 40.

The ionized sample 32 is supplied to the mass spectrometer 43
Then, the elements in the sample 32 and the concentrations of the respective elements are analyzed, and the analysis of the sample 32 is completed. Then, when analyzing a sample 32 ′ different from the sample 32, first, the four-way cock 63 of the cleaning means 60 is operated to another switching position. Then gas 5
2 is guided to the closed tank 61, the cleaning liquid 62 in the closed tank 61 is introduced into the spray chamber 36 through the blend gas line 51, the inside of the spray chamber 36 is cleaned, and the residual sample 32 is discharged through the drain hole 36a. It is discharged to the outside of the spray chamber 36 and stored in the drain tank 38.

Thereafter, the four-way cock 63 of the cleaning means 60 is returned to one of the switching positions, and the sample 32 'different from the sample 32 is analyzed. According to the above configuration, by flushing the residual sample 32 in the spray chamber 36 with the cleaning liquid 62, when performing the next analysis, it is necessary to introduce the sample 32 'until replacing the residual sample 32 of the previous analysis. The sample can be switched in a short time, and the sample can be saved.

Further, the cleaning liquid 62 is supplied to the spray chamber 3.
The cost can be reduced by sharing the line introduced into 6 and the blend gas line 51. Note that the present invention is not limited to the above embodiment. In the above embodiment, the cleaning liquid 62 is introduced into the spray chamber 36 using the blend gas line 51. However, an independent cleaning line is connected to the spray chamber 36, and the cleaning liquid is supplied to the spray chamber 36 by a pump or the like.
The spray chamber 36 may be introduced into the spray chamber 36 to clean the inside of the spray chamber 36.

(2) Second Embodiment FIG. 2 is a configuration diagram of a second embodiment of the present invention.
The difference between this embodiment and the first embodiment is only the cleaning means, and the other parts are the same.
In FIG. 1, the same parts as those in FIG. 1 are denoted by the same reference numerals, and the description thereof is omitted.

The first cleaning means 160 provided in the blend gas line 51 is provided with a first cleaning liquid (for example, pure water) 16.
2 is stored in the first closed tank 161 and the blend gas line 51. When the switch is switched to one position, the gas 52 flowing through the blend gas line 51 is passed straight, and when the switch is switched to the other position, the blend gas line is switched. The gas 52 flowing through the first closed tank 161 is introduced into the first closed tank 161 and the first cleaning liquid 162 in the first closed tank 161 is introduced.
And a first four-way cock 163 as switching means for sending out to the blend gas line 51.

In the blend gas line 51, the first
Second washing means 2 provided in series with the first washing means 160
Reference numeral 60 denotes a second closed tank 261 in which a second cleaning liquid (for example, nitric acid aqueous solution) 262 is stored, and a gas 52 which is provided in the blend gas line 51 and which flows through the blend gas line 51 when switched to one position. Straight through and switch to the other position, blend gas line 51
The gas 52 flowing through the second closed tank 261 is introduced into the second closed tank 261, and the second cleaning liquid 262 in the second closed tank 261 is sent to the blend gas line 51 by the second four-way cock 263 as a switching unit. It is configured.

In this embodiment, the cleaning liquid is used to attach the blend gas line 51 to the spray chamber 36.
And was provided so as to reach the end on the nebulizer 35 side. Next, the operation of the above configuration will be described. Nebulizer 3
5, a liquid sample 32 from a sample tank 31 and a carrier gas 34 are introduced via a gas flow controller 33, and the liquid sample 32 is atomized.

The atomized sample 32 is introduced into the spray chamber 36, and the mist having a large particle diameter among the atomized sample 32 is condensed and stored in the drain tank 38 through the drain hole 36a.

At this time, the first cleaning means 160 and the second
First and second four-way cocks 163 of the cleaning means 260
263 is switched to one position, and a gas 52 of the same or different type as the carrier gas 34 is introduced into the spray chamber 36 via the blend gas line 51.

The carrier gas 34 and the atomized sample 32
And a gas 52 of the same or different type as the carrier gas 34
The sample 32 is ionized by an inductively coupled plasma (ICP) 42 generated by a work coil 41 which is inserted into a plasma torch 39 and supplied with a current from a high frequency power supply 40.

At this time, the sample 3 to be ionized by the gas 52 of the same or different type as the carrier gas 34 is used.
2 is controlled. The ionized sample 32 is analyzed by the mass spectrometer 43 for the elements in the sample 32 and the concentration of each element, and the analysis of the sample 32 is completed.

When analyzing a sample 32 ′ different from the sample 32, first, the first 4
The side cock 163 is operated to another switching position. Then, the gas 52 is guided to the first closed tank 161, and the first cleaning liquid 162 in the first closed tank 161 is introduced into the spray chamber 36 through the blend gas line 51, and the inside of the spray chamber 36 is cleaned. And remaining sample 3
2 is the spray chamber 36 through the drain hole 36a.
It is discharged to the outside and stored in the drain tank 38.

Next, the first four-way cock 163 of the first cleaning means 160 is returned to one switching position, and the second four-way cock 263 of the second cleaning means 260 is operated to another switching position. . Then, the gas 52 is guided to the second closed tank 261 and the second cleaning liquid 16 in the second closed tank 261 is introduced.
2 is introduced into the spray chamber 36 through the blend gas line 51, the inside of the spray chamber 36 is washed, and the residual sample 32 is discharged out of the spray chamber 36 through the drain hole 36a.
Is stored in

Thereafter, the second cleaning means 260
The cock 263 is returned to the one switching position, and the sample 32 ′ different from the sample 32 is analyzed. In the above embodiment, the inside of the spray chamber 36 is cleaned with the first and second cleaning liquids 162 and 262 at the time of cleaning. However, the first cleaning liquid 162 is used depending on the type of the sample 32 or 32 '. And the type of the second cleaning liquid 163 may be selected and used properly.

According to the above configuration, the remaining sample 32 in the spray chamber 36 is washed out with the first and second cleaning liquids 162 and 262, so that the next time the next analysis is performed, the remaining sample 32 of the previous analysis is removed. Sample 32 'until replacement
This eliminates the need to introduce a sample, allows sample switching to be performed in a short time, and can save samples.

The first and second cleaning liquids 162, 26
The cost can be reduced by sharing the line for introducing 2 into the spray chamber 36 and the blend gas line 51.

After the residual sample 32 in the spray chamber 36 is washed away with the first cleaning liquid 62, the residual sample 32 in the spray chamber 36 is further rinsed with the second cleaning liquid.
By washing away, it is possible to further increase the washing effect as compared with the first embodiment.

[0044]

As described above, according to the first aspect of the present invention, a washing means for introducing a washing solution into the spray chamber is provided, and after the sample is analyzed, the remaining sample in the spray chamber is washed away with the washing solution. When performing the next analysis, there is no need to introduce a sample until the residual sample from the previous analysis is replaced, so that the sample can be switched in a short time and the sample can be saved.

According to the second aspect of the present invention, the cleaning means of the first aspect of the present invention can switch the sample in a very short time by cleaning the end on the nebulizer side. According to the invention of claim 3, in the invention of claim 1 or 2, the spray chamber is connected, and a blend gas line for introducing a gas of the same or different type as the carrier gas into the spray chamber is provided. The cleaning means is provided in a closed tank in which the cleaning liquid is stored, and in the blend gas line. When switched to one position, the gas flowing through the blend gas line passes straight through, and when switched to the other position, the blend gas flows. The gas flowing through the line is guided into the closed tank, and the switching means for sending the cleaning liquid in the closed tank to the blend gas line. Introduce the sample until replacing the residual sample from the previous analysis. This eliminates the necessity to use the sample, and allows the sample to be switched in a short time, and also allows the sample to be saved.

Further, the cost can be reduced by sharing the line for introducing the cleaning liquid into the spray chamber and the blend gas line. According to the fourth aspect of the present invention, the cleaning liquid according to any one of the first to third aspects is one of pure water and a water-soluble cleaning liquid. Switching can be performed quickly as compared with the above.

[Brief description of the drawings]

FIG. 1 is a configuration diagram of a first embodiment.

FIG. 2 is a configuration diagram of a second embodiment.

FIG. 3 is a configuration diagram of a conventional inductively coupled plasma mass spectrometer.

[Explanation of symbols]

 36 spray chamber 60 cleaning means

Claims (4)

[Claims] 1. A sample of a carrier gas and a liquid is introduced,
A nebulizer for atomizing the sample, and a spray chamber for introducing the atomized sample from the nebulizer, condensing the mist having a large particle diameter among the atomized samples, and discharging the condensate to the outside. An inductively coupled plasma mass spectrometer provided with a cleaning means for introducing a cleaning solution into the spray chamber. 2. The inductively coupled plasma mass spectrometer according to claim 1, wherein the cleaning means cleans the spray chamber up to the end on the nebulizer side. 3. A closed gas tank to which the spray chamber is connected, a blend gas line for introducing a gas of the same or different type as the carrier gas into the spray chamber is provided, It is provided in the blend gas line, and when it is switched to one position, the gas flowing through the blend gas line is passed straight through, and when it is switched to the other position, the gas that flows the blend gas is guided into the closed tank, and inside the closed tank. 3. An inductively coupled plasma mass spectrometer according to claim 1, further comprising: switching means for sending the cleaning liquid to the blend gas line. 4. The cleaning liquid according to claim 1, wherein the cleaning liquid is one of pure water and a water-soluble cleaning liquid.
The inductively coupled plasma mass spectrometer according to any one of the above.