JPH11326165A - Atomization introduction device of sample liquid - Google Patents

Abstract

PROBLEM TO BE SOLVED: To prevent the formation of the waterdrop and the reatomization phenomenon of a sample liquid to be measured that has been atomized by forming the inner space surface of an end cap formed between a nebulizer and a spray chamber with an ultra water-repellent material. SOLUTION: For example, an ultra-water-repellent part 52a where the surface of fluororesin is roughened by the air blast method or the like is provided on the surface of an inner space 52A of an end cap 52 that is formed between a front end 50a of a nebulizer 50 and a rear end (an opening end 51a of an outer pipe 51B) of a spray chamber 51. As a result, even if a sample to be measured being atomized by the neblizer 50 hits against the surface of the inner space 52A and becomes a waterdrop, the growth is prevented, thus avoiding the reatomization of the waterdrop at the front end 50a of the neblizer 50 and hence preventing spike noise or the like from being generated and achieving an analysis stably and reliably.

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

The present invention relates to a high frequency inductively coupled plasma / mass spectrometer (hereinafter referred to as ICP-MS) or a high frequency inductively coupled plasma / emission spectrometer (ICP-MS).
The present invention relates to an apparatus for introducing and atomizing a sample liquid used in an analyzer such as AES.

[0002]

2. Description of the Related Art FIG. 4 shows an example of the overall configuration of the ICP-MS. In the figure, reference numeral 1a denotes a sample tank for storing a solution to be measured, and 1b stores a solvent such as pure water. Tanks, 2a and 2b are pumps for sending out the solution to be measured and the solvent, 3 is a controller for controlling the amount of delivery of the pumps 2a and 2b, 4 is a computer for sending command signals to the controller, 5 is pumps 2a and 2b Nebulizer 500 and spray chamber 5 for atomizing the sample to be measured supplied from
A sample liquid atomizing and introducing device 10; 6 is an outermost tube 6a;
A plasma torch having, for example, a triple tube structure having an outer tube 6b and an inner tube 6c, 7a is an argon gas supply source, 7b is a pressure regulator for adjusting the pressure of the argon gas, 8 is a high frequency induction plasma, 9 is a high frequency induction coil, 10 Is a high frequency power supply for supplying high frequency energy to the high frequency induction coil 9;
1 is a nozzle, 12 is a skimmer, 13 is a fore chamber, 14 is a vacuum pump for sucking the interior of the fore chamber 13 to, for example, 1 Torr, 15 is a center chamber, 16
Is a vacuum pump that sucks the inside of the center chamber 15 to, for example, 10 ⁻² Torr, 17 is a pole such as a quadrupole mass filter, 18 is a rear chamber, and 19 is a suction to the rear chamber 18 to, for example, 10 ⁻⁴ Torr. A vacuum pump, 20 is a secondary electron multiplier, and 21 is a signal processing unit such as a microcomputer.

In the ICP-MS having such a configuration, the sample to be measured gasified by the sample liquid atomizing and introducing device 5 is supplied to the plasma torch 6 and is excited and ionized by the action of the high frequency induction plasma 8. The ionized sample to be measured is guided to the mass spectrometer via the nozzle 11 and the skimmer 12, where qualitative analysis and quantitative analysis are performed.

A specific configuration of the spray chamber 510 constituting the sample liquid atomizing and introducing apparatus 5 comprises an outer tube 511 and an inner tube 512, and an end cap 513 is attached to an open end of the outer tube 511, and the end cap is provided. The nebulizer 500 is attached via the attachment hole 513. In such a spray chamber 510, the measured sample atomized by the argon gas ejected from the spray holes of the nebulizer 500 passes through the inside of the inner tube 512 and the gap between the outer wall of the inner tube 512 and the inner wall of the outer tube 511. , Relatively large droplets (for example, water droplets having a diameter of 10 μm or more) are formed on the inner tube 5.
12 falls due to collision with the inner / outer wall 12 or the inner wall of the outer tube 511, and is discharged from the drain 514. The mist-like sample from which such large droplets have been removed is sent to the plasma torch 6 through the outlet pipe 515.

[0005]

However, in the above-described conventional atomization introducing device 5, when the sample to be measured atomized by the nebulizer 500 hits the inner surface of the end cap 513, water droplets and the like are generated. There was a phenomenon that the nebulizer 500 was drawn into the tip of the nebulizer 500 and atomized again. When such a re-atomization phenomenon occurs, there is a problem that a spike noise or the like is generated in a final detection signal, an error occurs in a measured value, and ultimately, stability and reliability of analysis are impaired.

SUMMARY OF THE INVENTION The present invention has been made to solve the above problems, and an object of the present invention is to provide an atomization introducing apparatus which can prevent re-atomization by a nebulizer, thereby improving the stability and reliability of analysis. And

[0007]

To achieve the above object, an atomizing introduction device according to the present invention comprises a nebulizer for atomizing a sample liquid to be measured and a sample to be measured atomized by the nebulizer. A spray chamber, and a nebulizer and an end cap to which the spray chamber is attached.
At least a surface of an inner space of the end cap formed between the nebulizer and the spray chamber is made of a super water-repellent material. According to the present invention, even if the measured sample atomized by the nebulizer hits the inner surface of the end cap and water droplets or the like are generated, the growth is prevented and the nebulization phenomenon by the nebulizer can be avoided.

In the present invention, the super-water-repellent material comprises:
It may be a fluororesin whose surface is roughened. Then, since the fluororesin is a known material, and various techniques for roughening the surface of the fluororesin, such as an air blast method of blowing abrasives with air, have been established, the surface of the inner space is super-repellent. An end cap made of an aqueous material can be easily manufactured.

In the above invention, the end cap may be made of a fluororesin, and the surface of the inner space may be roughened. By doing so, the trouble of forming a film made of fluororesin on the inner surface of the end cap made of a material other than fluororesin can be omitted.

In addition, instead of forming the surface of the inner space of the end cap from a super-water-repellent material, atomization introduction of a sample liquid provided with a linear member from the vicinity of the nebulizer tip to the lower end cap is provided. It may be a device.
According to this configuration, water droplets or the like generated on the inner surface of the end cap are not drawn into the tip of the nebulizer, but fall along the linear member as it is and fall on the end cap. Therefore, even in this configuration, the re-atomization phenomenon by the nebulizer can be prevented.

[0011]

DESCRIPTION OF THE PREFERRED EMBODIMENTS Embodiments of the present invention will be described below in detail with reference to FIGS. FIG. 1 is a side cross-sectional view of a sample liquid atomization introduction device according to an embodiment, FIG. 2 is a side cross-sectional view of an end cap of the atomization introduction device,
FIG. 3 is a side sectional view of a sample liquid atomization introduction device according to another embodiment.

As shown in FIG. 1, the sample liquid atomizing / introducing apparatus 5 includes an end cap 5 made of, for example, a fluororesin.
2, a nebulizer 50 and a spray chamber 51 having a double pipe structure are assembled so as to sandwich the nebulizer 50 therebetween. The inner surface of the end cap 52, that is, the surface of the inner space 52A formed between the front end 50a of the nebulizer 50 and the rear end of the spray chamber 51 (the open end 51a of the outer tube 51B), For example, a super-water-repellent portion 5 made of a super-water-repellent material having a roughened surface of a fluororesin
2a is provided.

As shown in FIG. 2, the end cap 52 is provided at its rear end with a nebulizer mounting portion 52b and a connector mounting portion 52c to which the nebulizer 50 and the blend gas connector 53 of FIG. 1 are screwed. A spray chamber mounting portion 52d into which the spray chamber 51 is fitted is provided on the front end side, and a
A connector mounting portion 52e to which the sample liquid introduction connector 54 is screwed is provided.

In FIG. 2, the inner space 52A of the end cap 52 gradually expands, for example, from the nebulizer mounting portion 52b to the spray chamber mounting portion 52d, and has the same inner diameter as the outer tube 51B of the spray chamber 51 in FIG. Spray chamber 51
The sample to be measured sprayed from the nebulizer 50 in FIG. 1 is introduced into the inner tube 51A.

The outer tube 51 of the spray chamber 51 shown in FIG.
B is attached to the end cap 52 in a watertight structure by a packing 52f provided in the spray chamber mounting portion 52d of the end cap 52.

According to the above embodiment, since the super-water-repellent portion 52a is provided on the surface of the inner space 52A of the end cap 52 in FIG. Hit the inside surface,
Even if water droplets are generated, their growth is prevented, and the re-atomization phenomenon of water droplets can be avoided, so that spike noise and the like can be prevented, and ultimately the stability and reliability of analysis are ensured. can do. Further, according to the above embodiment, the super water repellent portion 52a is made of a known fluororesin whose surface is roughened, and the surface is easily roughened to a desired state by an established technique such as an air blast method. Therefore, the end cap 52 in which the surface of the inner space 52A has super-water repellency can be easily manufactured. Furthermore, according to the above-described embodiment, since the end cap 52 itself is made of a fluororesin, the trouble of forming a film made of a fluororesin on the surface of the inner space 52A of the end cap 52 can be omitted.

The above embodiment can be variously modified. For example, the end cap 52 is formed of a material other than the fluororesin, a film of the fluororesin is formed on the surface of the inner space 52A, and the surface of the fluororesin film is subjected to the roughening treatment and the terminal by the fluorine gas as described above. The group may be subjected to carbon trifluoride (CF ₃ ) treatment. Further, the air cap 52 is connected to an air cap body,
The air cap body may be divided into a substantially conical trapezoidal portion which is attached later to the air cap body to form an inner space thereof and has an inner surface provided with a super water repellent portion 52a.

Next, based on FIG.
Of the sample liquid atomizing and introducing device provided with a linear member 55 extending from the vicinity of the front end of the nebulizer 50 to the lower end cap 52 in place of forming the surface of the inner space 52A of 2 in a super water-repellent material. The form will be described. Note that the same components as those of the above-described embodiment use the same reference numerals, and a detailed description thereof will be omitted. As shown in FIG.
One end of 5 is located immediately below the nebulizer front end 50a, and the other end faces the lower end cap 52.
The linear member 55 is, for example, a wire, and one end thereof may be adhered with an adhesive. According to such a configuration, even if water droplets and the like generated on the surface of the inner space 52A of the end cap 52 flow down to the vicinity of the nebulizer front end 50a, they are guided to the linear member 55 as they are,
From the lower end cap 52 to the inner tube 51A and the outer tube 51B
Is discharged from the drain 51C through the gap. Therefore, the re-atomization phenomenon by the nebulizer can be prevented.
Note that the mounting positions of both ends of the linear member 55 may be determined according to the arrangement of the front end of the nebulizer, and are not limited to the positions shown in FIG.

[0019]

According to the first aspect of the present invention, since at least the surface of the inner space of the end cap formed between the nebulizer and the spray chamber is made of a super-water-repellent material, the end cap is atomized by the nebulizer. Even if water droplets are generated due to the sample to be measured hitting the inner surface of the end cap, the growth is prevented, and the re-atomization phenomenon of the water droplets can be avoided. In addition, the stability and reliability of the analysis can be ensured.

According to the second aspect of the present invention, since the surface of the inner space of the end cap made of fluororesin is roughened, the inner surface of the end cap made of a material other than fluororesin is coated with fluororesin. There is an advantage that the trouble of forming a film can be saved.

According to the third aspect of the present invention, water droplets and the like generated on the inner surface of the end cap are not drawn into the tip of the nebulizer, but are directly transmitted through the linear member and fall on the end cap. Therefore, even in this configuration, the re-atomization phenomenon by the nebulizer can be prevented.

[Brief description of the drawings]

FIG. 1 is a side cross-sectional view showing an embodiment of a sample liquid atomization introduction device according to an embodiment.

FIG. 2 is a side sectional view of an end cap used in the sample liquid atomizing and introducing apparatus according to the present invention.

FIG. 3 is a side sectional view showing an embodiment of a sample liquid atomization introduction apparatus according to another embodiment.

FIG. 4 is an overall configuration diagram of an ICP-MS showing an example of an apparatus using an apparatus for introducing and atomizing a sample liquid.

[Explanation of symbols]

 Reference Signs List 5 atomization introduction device for sample liquid 6 plasma torch 50,500 nebulizer 50a front end of nebulizer 51,510 spray chamber 51B, 511 outer tube 51a open end of outer tube 51A, 512 inner tube 52,513 end cap 52A inside of end cap Space 52a Super water-repellent part 52b Nebulizer mounting part 52c Connector mounting part 52d Spray chamber mounting part 52e Connector mounting part 53 Blend gas connector 54 Connector for sample liquid introduction 55 Linear member 51C 514 Drain 515 Outgoing pipe

Continued on the front page (72) Inventor Shuzo Nagaoka 1-15-5 Nakamachi, Musashino-shi, Tokyo Mitaka Takagi Building Yokogawa Analytical Systems Co., Ltd.

Claims (3)

[Claims] A nebulizer for atomizing a sample liquid to be measured;
A spray chamber into which a sample to be measured atomized by the nebulizer is introduced, and a nebulizer and an end cap to which the spray chamber is attached, the sample liquid atomization introduction device, wherein the end cap, at least the nebulizer and An apparatus for atomizing and introducing a sample liquid, wherein a surface of an inner space formed between the spray chamber and the spray chamber is made of a superhydrophobic material. 2. The device for atomizing and introducing a sample liquid according to claim 1, wherein the end cap is made of a fluororesin, and a surface of an inner space thereof is roughened. 3. A nebulizer for atomizing a sample liquid to be measured,
In a device for atomizing and introducing a sample liquid comprising a spray chamber into which a sample to be measured atomized by the nebulizer is introduced, and an end cap to which the nebulizer and the spray chamber are attached, the lower end from near the tip of the nebulizer. An atomizing introduction device for a sample liquid, comprising a linear member facing a cap.