JPH0619077Y2 - Sample melting reaction vessel for high frequency heating - Google Patents

Description

[Detailed description of the device] [Industrial application field] The present invention is for chemical analysis (qualitative analysis, quantitative analysis, colorimetric analysis).
The present invention relates to a high-frequency heating sample dissolution reaction container for preliminarily dissolving a target sample in a solvent by the chemical analysis.

[Prior Art] A sample dissolution reaction container proposed by the present applicant and disclosed in Japanese Utility Model Laid-Open No. 62-37743 discloses a synthetic resin inner container for accommodating a sample and a solvent therein, and the inner container. It is composed of a metal outer container that is housed and held in a sealed state.

[Problems to be Solved by the Invention] According to the above sample dissolution reaction container, the dissolution reaction of the sample in the inner container can be completed in a short time at high temperature and high pressure.

However, the heating time required to reach the high temperature required to accelerate the dissolution reaction of the sample in the inner container and the cooling time required to return to normal temperature after the completion of the dissolution reaction are relatively long and required several tens of minutes to 1 hour or more. .

An object of the present invention is to shorten the heating time and cooling time of the sample in the inner container by further improving the sample dissolution reaction container.

[Means for Solving Problems] A sample melting reaction container for high-frequency heating according to the present invention comprises a bottomed outer cylinder having an opening at the top and a detachable outer lid at the top of the outer cylinder. An outer container made of a material with a low dielectric constant, a bottomed inner cylinder that has a seating surface on the top and contains the sample inside,
An inner container made of a synthetic resin that is seated on the seating surface and has a mating surface that holds the inside of the bottomed inner cylinder in a hermetically sealed state, and is housed in the outer container and pressed to keep the hermetically sealed state. In the reaction container, the outer peripheral surface of the lower portion of the outer cylinder is formed with a pair of parallel engaging surfaces sandwiched by a fixed tool, and the outer lid is engaged with the engaging tool for engaging the tightening tool. A mating portion is formed, the inner container is housed in the outer cylinder having a pair of parallel engagement surfaces sandwiched and fixed by the fixing tool, and the outer lid is engaged with the outer cylinder. By tightening the outer lid with a tightening tool engaged with the engaging portion of the outer lid, the inner lid is crimped to the bottomed inner cylinder and the sealed state of the bottomed inner cylinder is maintained. By irradiating a high frequency from the outside through the outer container, the sample in the inner container can be directly heated. It is an butterfly.

According to such a sample melting reaction container for high frequency heating, the sample in the inner container can be directly heated by irradiating the high frequency from the outside through the outer container, so that the time required to reach the high temperature necessary for the dissolution reaction is significantly increased. Shortened. Further, after the dissolution reaction of the sample at the high temperature, at least the outer cylinder is not heated, so that the sample can be cooled in a short time by stopping the irradiation of the high frequency. .

The sample melting reaction container for high frequency heating of the present invention comprises an outer container,
The inner container is a component.

The outer container is made of a material having a low dielectric constant, accommodates the inner container inside, and supports the outer periphery of the inner container. The outer container is formed of a bottomed outer cylinder having an opening at the top and a detachable outer lid on the top of the outer cylinder. Further, in order to make the outer lid attachable to and detachable from the upper portion of the outer cylinder, screwing or fitting, press contacting or other means can be used. Also, the outer cylinder is the cylinder body,
A removable bottom portion can be used for the inner peripheral bottom portion of the cylinder body.

In this case, when the solvent adheres to the inside of the outer container, the bottom of the outer container can be removed to easily clean the inside of the outer container and the removed bottom.

In addition, the material with a low dielectric constant that constitutes the outer container has a dielectric constant of 1
Structural materials of 0.0 or less can be used. As such a structural material, synthetic resins such as polypropylene and polycarbonate, and ceramics such as alumina and magnesia can be used.

Further, it is desirable that the male screw and the female screw, which are formed on the outer lid and the outer cylinder of the outer container and engage with each other by screwing, are made of different materials. For example, one of the male screw and the female screw can be made of polypropylene, and the other of the male screw and the female screw can be made of polycarbonate. In this case, the male screw and the female screw can be prevented from being melted and integrated with each other in a screw-engaged state.

The inner container is fluororesin, chlorinated polyether, allyl resin,
Inner cylinder with a bottom that has a seating surface on the top made of synthetic resin that has chemical resistance and heat resistance such as polyallylsulfone and polymethylpentene, and the inner surface of the bottomed inner cylinder that is seated on the seating surface and is kept sealed It is formed of an inner lid having a mating surface and is housed in an outer container to maintain a sealed state.

[Operation] The inner container, in which the sample and the solvent are housed, is housed in the outer cylinder in which the pair of parallel engagement surfaces are sandwiched and fixed by the fixing tool. After that, the outer lid is engaged with the outer cylinder, and the inner lid is crimped to the bottomed inner cylinder by tightening the outer lid with the tightening tool engaged with the engaging portion of the outer lid. The sealed state of the inner cylinder is maintained. Along with this, the outer periphery of the inner container is supported by the outer container.

In this state, the sample in the inner container is directly heated by radiating a high frequency from the outside through the outer container.

[Effect] When tightening the outer lid with the tightening tool, the outer cylinder holds the pair of parallel engaging surfaces by the fixing tool, so that the outer lid and the outer cylinder can be tightened more firmly. ,
Moreover, the inner lid can be securely crimped to the bottomed inner cylinder, and the degree of sealing can be enhanced.

Further, since the outer container is made of a material having a low relative dielectric constant, the sample in the inner container can be directly heated without being heated during the irradiation with the high frequency.

Therefore, the heating time required to reach the high temperature necessary for the dissolution reaction of the sample can be shortened as compared with the case where the sample is heated through the reaction vessel. Further, if the heating of the sample by irradiation of the high frequency is stopped at the time when the dissolution reaction of the sample is completed, the reaction container, particularly the outer cylinder is not heated, so that the sample can be cooled in an extremely short time.

[Example] Example 1 of the sample dissolution reaction container for high frequency heating of the present invention,
Description will be given based on FIG. 1 shown in a perspective view and FIG. 2 shown in cross section.

The sample melting reaction container for high frequency heating of this embodiment has an outer container 1 and an inner container 2 made of a material having a low relative dielectric constant as constituent elements.

The outer container 1 is composed of a bottomed outer cylinder 10 made of polypropylene and having a relative dielectric constant of 3.0 or less, which is not heated by being irradiated with a high frequency (frequency 2457 MHz ± 50 Hz), and an outer lid 11 made of polycarbonate. There is.

The outer cylinder 10 includes a cylinder body 100 and a bottom portion 102 that is detachably engaged with an annular engagement portion 101 formed on the inner peripheral bottom portion thereof.
It consists of and. A male screw 103 is formed on the outer periphery of the upper portion of the outer cylinder 10. Further, on the outer peripheral surface of the lower portion of the outer cylinder 10, a pair of parallel engagement surfaces 10 sandwiched by the fixed tool 1A.
4, 105 are formed. At the center of the outer lid 11,
A central hole 111 for reducing the contact area is formed so that the tightening force is uniformly applied to the inner lid 21 of the inner container 2. Further, a female screw 110 that is screw-engaged with the male screw 103 of the outer cylinder 10 is formed on the inner periphery of the lower portion of the outer lid 11.
Further, the lid 11 is formed with an engaging portion 112 for engaging the tightening tool 1B.

The inner container 2 includes a bottomed inner cylinder 20 made of fluororesin having chemical resistance and heat resistance, and an inner lid 21. A seating surface 201 is formed on the top of the bottomed inner cylinder 20. Inner lid 2
In the lower part of 1, there is a mating surface 211 that sits on the seating surface 201.
Are formed. A cross-sectional inclination angle between the seating surface 201 and the mating surface 211 is about 30 °.

Next, the operation of this embodiment configured as described above will be described.

A sample A (for example, plant fiber) to be melted is put in a bottomed inner cylinder 20 made of fluororesin together with a dissolved chemical liquid B (for example, nitric acid). The bottomed inner cylinder 20 is housed in the outer cylinder 10 in which the engaging surfaces 104 and 105 are sandwiched and fixed by the fixing tool 1A. Next, the mating surface 211 of the inner lid 21 is seated on the seating surface 201 of the bottomed inner cylinder 20. Then, the outer lid 11 is screwed into the outer cylinder 10. The outer lid 11 is an engaging portion 11
The tightening tool 1B engaged with 2 is rotated in the direction of the arrow, whereby the tightening is further tightened.

The outer lid 11 presses the inner lid 21 so that the mating surface 2
11 is closely attached to the seating surface 201. Therefore, the inside of the inner container 2 is sealed. The outer periphery of the inner container 2 is supported by the outer container 1.

The sample melting reaction container for high frequency heating in this state is set in a high frequency heating device (not shown). Next, the sample melting reaction container for high frequency heating is irradiated with high frequency from the outside through the outer container 1. Then, the sample A and the dissolved chemical liquid B in the inner container 2 are directly heated, and the irradiation heating time of about several minutes is about 1
A heating temperature of 10 ° C. is reached. This heating temperature is maintained by subsequent irradiation with high frequency. Alternatively, it is held by the heat of reaction. As a result, in the inner container 2, the dissolution reaction of the sample A by the dissolved chemical liquid B is promoted. Moreover, the dissolution reaction of the sample A at a high temperature can be completed in about 8 minutes.

As described above, according to the sample melting reaction container for high frequency heating of the present invention, the outer container 1 made of a material having a low relative dielectric constant is not heated to a high temperature when irradiated with a high frequency. Therefore, the sample A and the dissolved chemical liquid B in the inner container 2 can be heated to the high temperature required for the dissolution reaction in a short time. Further, after the high frequency irradiation is stopped and the sample is completely dissolved, the outer container is not heated, so that the container can be immediately touched and taken out to start the next analysis step, so that the whole working time can be greatly shortened. Further, since the outer cylinder 10 and the outer lid 11 which are screw-engaged with each other are not heated to a high temperature, the male screw 103 and the female screw 110 are not thermally deformed and fused, and the sealed state of the inner container 2 is maintained and the melting is performed. Allow the reaction to finish smoothly.

Therefore, the dissolved sample required for chemical analysis can be obtained in an extremely short time.

[Embodiment 2] FIG. 3 shows Embodiment 2 of the sample melting reaction container for high frequency heating of the present invention.

In this embodiment, a female screw 103a is formed on the upper inner peripheral surface of the outer cylinder 10a.
Is formed.

The outer lid 11a has a substantially columnar shape, and a male screw 110a that is screwed into the female screw 103a is formed on the central outer peripheral portion.

Further, the outer lid 11a has two through holes 111a and 112a penetrating horizontally in a cross shape in the upper portion thereof.
It is used as the engaging portion of B.

Other configurations and effects of the present embodiment are similar to those of the first embodiment, and therefore description thereof will be omitted. The same components as those in the first embodiment are designated by the common reference numerals.

[Embodiment 3] FIG. 5 shows Embodiment 3 of the sample melting reaction container for high frequency heating of the present invention.

This embodiment has the same configuration as that of the first embodiment except that it has a rectangular central hole 11a formed in the central portion of the outer lid 11.

In the case of this embodiment, instead of the tightening tool 1B of the first embodiment,
By engaging the tightening tool 1C with the central hole 11a, the outer lid 11
Can be tightened in the direction of the arrow. That is, while engaging the adapter 11c with the central hole 11a,
Torque wrench body 12c engaged with adapter 11c
A constant tightening force can always be obtained by tightening by, and the pressing force of the inner lid 21 by the outer lid 11 and the degree of sealing of the inner lid 21 do not vary among the tightening operators.

[Brief description of drawings]

1 and 2 are explanatory views of a sample melting reaction vessel for high-frequency heating according to Embodiment 1 of the present invention, FIG. 1 is an exploded perspective view showing a main part, and FIG. 2 is a longitudinal sectional view showing a use state. Is. FIG. 3 is a longitudinal sectional view showing a sample melting reaction container for high frequency heating according to a second embodiment of the present invention. FIG. 4 shows the outer lid 11a in FIG.
FIG. FIG. 5 is a vertical cross-sectional view showing a sample melting reaction container for high frequency heating according to a third embodiment of the present invention. DESCRIPTION OF SYMBOLS 1 ... Outer container, 10 and 10a ... Outer cylinder 11, 11a ... Outer lid, 100 ... Tube body 101 ... Annular locking part, 102 ... Bottom 103, 110a ... Male screw 110, 103a. Internal thread 2 ... Inner container, 20 ... Inner cylinder with bottom 21 ... Inner lid, 201 ... Seating surface 211 ... Mating surface, A ... Sample B ... Dissolved chemical liquid

Claims (3)

[Scope of utility model registration request] 1. An outer container made of a material having a low relative dielectric constant, which is composed of a bottomed outer cylinder having an opening at the top and a detachable outer lid at the top of the outer cylinder, and a seating surface at the top. A bottomed inner cylinder for accommodating a sample therein, and an inner lid having a mating surface that sits on the seating surface and holds the inside of the bottomed inner cylinder in a sealed state, and is accommodated in the outer container In a reaction container comprising an inner container made of a synthetic resin that is pressed to maintain a closed state, a pair of parallel engaging surfaces to be held by a fixed tool is formed on a lower outer peripheral surface of the outer cylinder, An engaging portion for engaging a tightening tool is formed on the outer lid, and the inner container is housed in the outer cylinder having a pair of parallel engaging surfaces sandwiched and fixed by the fixing tool. At the same time, the outer lid is engaged with the outer cylinder, and the outer lid is retightened by a tightening tool engaged with the engaging portion of the outer lid. The inner lid is crimped to the bottomed inner cylinder to keep the bottomed inner cylinder in a sealed state, and the sample in the inner container can be directly heated by radiating a high frequency from the outside through the outer container. A sample dissolution reaction container for high-frequency heating, characterized in that 2. A sample melting reaction container for high-frequency heating according to claim 1, wherein the outer lid and the outer cylinder are screw-engaged with each other, and the outer cylinder has a removable bottom. 3. The sample melting reaction for high frequency heating according to claim 1, wherein the material of the outer container having a low dielectric constant is a ceramic material or a synthetic resin material having a dielectric constant of 10.0 or less. container.