WO2005054813A1 - Microwave heating-purpose sample decomposition reaction vessel - Google Patents

Abstract

An object of he invention is to provide a decomposition reaction vessel adapted for microwave decomposition method and allowing visual observation of a sample in the process of reaction from outside and being capable of being used for every microwave generating device without being deformed. As a solving means therefor, it comprises an outer vessel of metal consisting of an outer sleeve having a plurality of slits cut therein and an outer lid removably threadedly fitted to the top of the outer sleeve, and an inner vessel consisting of a bottomed semitransparent inner sleeve and an inner lid seated on the top of the inner sleeve, wherein the inner sleeve is stored in the outer vessel with its outer peripheral surface being in close contact with the inner peripheral surface of the outer sleeve, the inner sleeve and inner lid being pressed by a pressing means so that the interior of the inner vessel is held in a hermetically closed state.

Description

 Specification

 Sample decomposition reaction vessel for microwave heating

 Technical field

 The present invention relates to a sample decomposition reaction vessel for microwave heating for dissolving or reacting a sample to be subjected to chemical analysis such as qualitative analysis or quantitative analysis in advance with a reagent such as a solvent or an acid.

 Background art

 [0002] As a pretreatment for quantifying and qualifying components in a sample, a sample and a reagent such as a solvent or an acid (hereinafter referred to as "solvent") are placed in a decomposition reaction vessel to accelerate the reaction under high temperature and high pressure. The sample must be decomposed or reacted.

 As a decomposition reaction vessel, a decomposition reaction vessel disclosed in Japanese Utility Model Publication No. 4-16924 is known. FIG. 8 is an exploded perspective view of a decomposition reactor disclosed in Japanese Utility Model Publication No. Hei 4-16924. As shown in FIG. 8, the decomposition reaction vessel 100 has a stainless steel outer vessel 110 and a synthetic resin An inner container 120, a pressing member 130 made of stainless steel, and a pressing member 140 made of stainless steel bolts.

 However, in recent years, it has been desired to create a high-temperature and high-pressure state by microwave irradiation, which is often used to further shorten the reaction time, but since the decomposition reaction vessel 100 is covered with stainless steel, The microwave is attenuated by the reflection on the stainless steel surface of the decomposition reaction vessel 100 and the absorption inside the stainless steel, so that a high-temperature and high-pressure state cannot be created, and the sample and solvent in the inner container 120 are heated. I can't.

 [0003] On the other hand, as a decomposition reaction vessel compatible with the microwave decomposition method, the one shown in FIG. 9 is known. In FIG. 9, the decomposition reaction vessel 200 is composed of a bottomed cylinder 210 having an opening at the top, and a detachable outer lid 220 at the top of the cylinder, and a pressure regulating valve 230 is provided at the upper part of the outer lid 220. Has been installed. When the pressure in the decomposition reaction vessel 200 exceeds a predetermined value, the pressure regulating valve 230 operates to release the gas in the decomposition reaction vessel 200 to a collection vessel (not shown), thereby preventing deformation and explosion of the vessel. .

[0004] Further, the reaction vessel disclosed in Japanese Utility Model Publication No. 6-19077 shown in FIG. It corresponds to. FIG. 10 is an exploded perspective view of the one disclosed in Japanese Utility Model Publication No. 6-19077. As shown in FIG. 10, the reaction vessel 300 has a bottomed outer cylinder 310 having an opening at the top, and the outer cylinder 310. An outer container 310 made of a material having a low relative dielectric constant and having a detachable outer lid 320 at the upper part of the outer container 310; a bottomed inner cylinder 322 having a seating surface 321 at the upper part and containing a sample therein; An inner lid 323 having a mating surface which is seated on a seating surface and holds the inside of the bottomed inner cylinder in a sealed state, and which is housed in the outer container 310 and pressed to maintain a sealed state by a synthetic resin inner container 320. It consists of:

[0005] In the reaction container 300, since the outer container 310 is made of a material having a low relative dielectric constant and the inner container 320 is also made of a synthetic resin, microwaves are not attenuated inside the inner container 320. Samples and solvents can be heated.

 Patent Literature 1: Jitsuhei 4-1-1 16924

 Patent Document 2: Jitsuhei 6-19077

 Disclosure of the invention

 Problems to be solved by the invention

 [0006] As described above, in the decomposition reaction vessel 200, since the pressure of the vessel is required, the wall of the vessel has a predetermined thickness, and thus must be opaque. Requires a special microwave generator with a special structure that allows the gas in the reaction vessel to escape to the collection vessel, and cannot be used for other microwave generators. No versatility. In the reaction container 300, the reaction container 300 has a double structure, and the sample in the inner container 320 cannot be visually observed through the outer container 310 and the inner container 320. Therefore, since the reaction process of the sample cannot be seen from the outside, it is difficult to judge the completion of decomposition until it is opened.

 [0007] Therefore, the present invention can be used for a heating vessel and a heating reaction vessel and also supports a microwave decomposition method, so that a sample in the course of the reaction can be visually observed from the outside and is not deformed. An object of the present invention is to provide a decomposition reaction vessel that can be used also in a microwave generator such as a microwave oven used in the above.

 Means for solving the problem

[0008] In order to solve the above problems, the sample decomposition reaction vessel for microwave heating according to claim 1 Are an outer cylinder provided with a plurality of slits, an outer container serving as an outer lid detachably screwed onto the upper part of the outer cylinder, and an inner container or bottom having a translucent inner cylinder having a bottom. An inner container comprising a translucent inner cylinder and an inner lid seated on the upper part of the inner cylinder, wherein the outer peripheral surface of the inner cylinder is in close contact with the inner peripheral surface of the outer cylinder to the outer container. The inner tube and the outer lid are housed and pressed by pressing means, or the inner tube and the inner lid are pressed by pressing means, whereby the interior of the inner container is maintained in a sealed state. I have.

 Further, the sample decomposition reaction container for microwave heating according to claim 2 is the sample decomposition reaction container for microwave mouth wave heating according to claim 1, wherein the outer cylinder and the outer lid are made of stainless steel, alumina, A material made of at least one or a combination of a sintered body and a polyimide resin (trade name: Vespel (“Vespel” is a registered trademark of DuPont)), and the inner cylinder is made of glass, quartz glass, or fluorine. One of chemical modified polyethylene propylene resin (trade name: Teflon F EP (“Teflon” is a registered trademark of DuPont)) or perfluoroalkoxy resin (trade name: Teflon PFA (“Teflon” is a registered trademark of DuPont)) Or a combination of two or more, and the inner lid is made of fluorinated polyethylene propylene resin, ethylene tetrafluoride resin or perfluoroalkoxy resin. Les, as characterized by a material consisting of one or more combinations of Ru.

The microwave heating sample decomposition reaction container according to claim 3 is the microwave heating sample decomposition reaction container according to claim 1 or claim 2, wherein the inner container is pressed by the pressing means. A gas discharge unit that allows communication between the inside of the inner container and the outside of the outer container in a closed state.

Further, the sample decomposition reaction container for microwave heating according to claim 4 is the sample decomposition reaction container for microwave heating according to claim 1 to claim 3, wherein the pressing means has the outer lid. The gas discharge unit is configured to be pressed by being screwed into the outer cylinder, and the gas discharge unit is provided with a first flow passage formed in a center portion of the outer lid and vertically penetrated, and penetrates vertically. And a flow passage opening / closing bolt having a second flow passage and screwed into the outer lid. The gas flow passage is shut off by bringing the lower end of the flow passage opening / closing bolt into close contact with the outer lid surface. The gas flow passage is formed by separating the lower end of the flow passage opening / closing bolt from the outer lid surface. Further, the sample decomposition reaction container for microwave heating according to claim 5 is the sample decomposition reaction container for microwave heating according to claims 1 to 3, wherein the pressing means is provided at a central portion of the outer lid. The gas discharge means is configured to be pressed by a pressurized bolt screwed into the inner lid, and the gas discharge means is provided with a first flow passage penetrated in a vertical direction formed in a center portion of the inner lid, and a first flow passage penetrated in a vertical direction. A flow passage opening / closing bolt which has two flow passages and is screwed into the inner cover through the outer cover, and a lower end of the flow passage opening / closing bolt is brought into close contact with the inner cover surface. The gas flow passage is shut off, and the gas flow passage is formed by separating the lower end of the flow passage opening / closing bolt from the inner lid surface. The microwave heating sample decomposition reaction vessel according to claim 6 is the microwave heating sample decomposition reaction vessel according to claims 1 to 5, wherein an annular shape is provided inside the upper part of the outer cylinder. A step is formed, and a flange formed at an upper portion of the inner cylinder is fitted to the step, and the inner container is fixed to the outer container.

 Furthermore, the sample decomposition reaction container for microwave heating according to claim 7 of the present application is the sample decomposition reaction container for microwave heating according to claim 1 or claim 6, wherein the outer cylinder is an annular step inside. An upper outer cylinder having a portion formed therein and a lower outer cylinder having a plurality of slits formed therein, wherein the upper outer cylinder and the lower outer cylinder are detachably screwed to each other.

 The invention's effect

 [0010] In the sample decomposition reaction container for microwave heating according to claim 1 of the present application, since the outer container provided with a plurality of slits and the inner cylinder are constituted by a translucent inner container, the microphone is passed through the slits. The mouth wave reaches the translucent inner container without being attenuated, and can heat the sample and the solvent in the inner container. Then, the sample during the reaction process in the inner container can be visually observed from the outside through the slit.

 In addition, since the outside of the inner cylinder of the inner container is housed in close contact with the inside of the outer cylinder of the outer container, even if a tensile stress acts on the inner cylinder of the inner container due to an increase in the internal pressure during thermal decomposition, the pulling is performed Since the outer container bears the tensile stress, the inner container is not deformed.

[0011] In the sample decomposition reaction container for microwave heating according to claim 2, the outer cylinder constituting the outer container is formed of one or more of stainless steel, alumina sintered body, or polyimide resin. The outer lid is made of stainless steel or one of alumina sintered bodies or a combination of these, and the inner cylinder that constitutes the inner container is made of glass, quartz glass, fluorinated polyethylene propylene resin or perfluorocarbon. The inner lid is made of one of the alkoxy resins or a combination thereof, and the inner lid is made of a fluorinated titanium propylene resin, a tetrafluorinated ethylene resin, or a perfluoroalkoxy resin. When the outer container is made of a metal, stainless steel, a Hastelloy alloy, or an anolemina sintered body is preferred because a metal having high corrosion resistance is preferred. A stainless steel or an alumina sintered body is more preferable in terms of workability. When the outer container is made of a polyimide resin, the outer container can be made lighter than when it is made of a metal.

 Further, since the inner cylinder of the inner container needs to have chemical resistance, heat resistance and transparency, it is preferable to be made of glass, quartz glass or perfluoroalkoxy resin.

 [0012] The sample decomposition reaction container for microwave heating according to claim 3 is provided with gas discharge means that enables communication between the inside of the inner container and the outside of the outer container when the inner container is pressed. Therefore, after heating the sample decomposition reaction container for microwave heating, the gas generated in the inner container by the reaction of the sample is exhausted in advance to reduce the pressure in the inner container, which is at a high pressure. In addition, it is possible to prevent ejection of the sample after the reaction.

 [0013] Further, the sample decomposition reaction container for microwave heating according to claim 4 or claim 5 is configured such that the gas discharge passage constituting the gas discharge means is open at the top and penetrates into the inner container. Because it is provided, by connecting a hose with one end connected to the gas analyzer to the open part with the upper part opened, the gas component analysis after heating the sample decomposition reaction vessel for microwave heating is performed If the evolved gas is poisonous as much as possible, a collector can be connected to the opening to prevent diffusion of the poisonous gas to the outside.

 Even after the sample is placed in the inner container and the sample decomposition reaction vessel for microwave heating is set, if the flow passage opening / closing bolt is removed, the upper and lower holes drilled in the center of the outer lid or inner lid are removed. The first flow path force penetrating in the direction The injector such as a syringe enables additional injection of a solvent or the like, so-called pouring.

[0014] The sample decomposition reaction vessel for microwave heating according to claim 6 is provided inside the upper part of the outer cylinder. The flange formed on the upper outer side of the inner cylinder is fitted and fixed to the step formed on the inner container, so that the inner container can be easily attached to and detached from the outer container.

 Further, in the sample decomposition reaction vessel for microwave heating according to claim 6, since the outer cylinder is separate from the upper outer cylinder and the lower outer cylinder, only the height can be changed without changing the diameter of the inner cylinder of the inner container. Therefore, various inner containers with different contents can be handled by changing only the height of the lower outer cylinder without changing the shapes of the outer lid and the upper outer cylinder that constitute the outer container. Become. Furthermore, since the outer cylinder is separate from the upper outer cylinder and the lower outer cylinder and is screwed removably, it is taken out of the microwave generator and cooled down to the point where the upper and lower outer cylinders are touched by hand. Only the tube can be removed, and the contents of the inner container can be checked before completely cooling.

Brief Description of Drawings

FIG. 1 is an exploded perspective view of a sample decomposition reaction vessel for microwave heating according to Example 1.

 FIG. 2 is a diagram showing a microwave generator and a sample decomposition reaction container for microwave heating according to Example 1 housed in the microwave generator.

 FIG. 3 is a view showing a sample decomposition reaction vessel for microwave heating according to Example 1 irradiated with microwaves.

 FIG. 4 is an exploded perspective view of a sample decomposition reaction container for microwave heating according to Example 2.

 FIG. 5 is an assembled sectional view of a sample decomposition reaction container for microwave heating according to Example 2.

 FIG. 6 is an explanatory cross-sectional view for collecting generated gas in an inner container of a sample decomposition reaction container for microwave heating according to Example 2.

 FIG. 7 is an assembled sectional view of a sample decomposition reaction container for microwave heating according to Example 3.

 FIG. 8 is an exploded perspective view of a decomposition reactor disclosed in Japanese Utility Model Publication No. Hei 11-16924.

[FIG. 9] FIG. 9 shows a microwave generator and a conventional purf housed in the microwave generator. It is a figure showing a decomposition reaction vessel made of a loroalkoxy resin.

 FIG. 10 is an exploded perspective view of the one disclosed in Japanese Utility Model Publication No. 6-19077. Explanation of symbols

10 Microwave heating sample decomposition reaction vessel according to Example 1

12 Microwave heating sample decomposition reaction vessel according to Example 2

14 Microwave heating sample decomposition reaction vessel according to Example 3

20 Outer container according to Example 1 and Example 2

20c Outer container according to Example 3

21a Outer lid according to Example 1

21b Outer lid according to Example 2

21c Outer lid according to Example 3

23a Outer cylinder according to Example 1

23b Outer cylinder according to Example 2

23c Outer cylinder according to Example 3

24 Upper outer cylinder

25 Lower outer cylinder

28 Bottom outer cylinder

30 inner container

 31a Inner lid according to Example 1

31b Inner lid according to Example 2

33 inner cylinder

 37 Conical protrusions

 38 Packing body

 1a Pressure Bolt According to Example 1

 1b Pressure bolt according to Example 2

 2a Pressing plate according to Example 1

 2b Press plate according to Example 2

3 Buffer ring 72 Flow passage opening / closing bolt

 75 First flow passage according to Example 2

 76 First flow passage according to Example 3

 77 2nd passage

 78 Flow passage space

 BEST MODE FOR CARRYING OUT THE INVENTION

 [0017]

 Example 1

 Example 1 of a sample decomposition reaction vessel for microwave heating according to the best mode for carrying out the present invention will be described in detail with reference to FIGS. 1 to 3. Fig. 1 is an exploded perspective view of a sample decomposition reaction vessel for microwave heating according to Example 1, and Fig. 2 is a microwave generator and a sample for microwave heating according to Example 1 housed in the microwave generator. FIG. 3 is a view showing a sample decomposition reaction container for microwave heating according to Example 1 irradiated with microwaves.

 First, the configuration of the sample decomposition reaction container for microwave heating according to Example 1 will be described with reference to FIG. 1, reference numeral 10 denotes a sample decomposition reaction vessel for microwave heating according to Example 1, reference numeral 20 denotes an outer container, reference numeral 21a denotes an outer lid of the outer container 20, and reference numeral 22 denotes a central portion of the outer lid 21a. Reference numeral 23a denotes an outer cylinder of the outer container 20, reference numeral 24 denotes an upper outer cylinder constituting the outer cylinder 23a, and reference numeral 25 denotes a lower outer cylinder constituting the outer cylinder 23a. Reference numeral 30 denotes an inner container, reference numeral 31a denotes an inner lid of the inner container 30, and reference numeral 33 denotes a bottomed inner cylinder. Reference numeral 41a denotes a pressure bolt, reference numeral 42a denotes a pressing plate, and reference numeral 43 denotes a buffer ring. In this embodiment, the outer container 20 is made of stainless steel or alumina sintered body. Although a plurality of slits are formed in the lower outer cylinder 25 constituting the outer container 20, in the present embodiment, vertically long slits 27a and three-stage horizontally long slits 27b are alternately provided. A female screw is threaded on the upper inner peripheral surface of the lower outer cylinder 25, and is removably screwed with a male screw threaded on the lower outer peripheral surface of the upper outer cylinder 24.

[0020] The inner diameter of the upper outer cylinder 24 is formed to be the same as the inner diameter of the lower outer cylinder 25, but the upper part of the upper outer cylinder 24 is formed larger than the inner diameter of the lower outer cylinder 25. 26 is shape Made. A male screw is threaded on the upper outer peripheral surface of the upper outer cylinder 24, and is removably screwed to a female screw threaded on the lower inner peripheral surface of the outer lid 21a.

 The inner container 30 includes a bottomed inner cylinder 33 made of perfluoroalkoxy resin having chemical resistance and heat resistance, and an inner lid 31a. A seating surface 34 is formed at an upper portion of the inner cylinder 33, and a mating surface 32 which is seated on the seating surface 34 is formed at a lower portion of the inner lid 31a. The wall thickness of the inner cylinder 33 is set to 5 mm in order to make it semi-transparent.

 Next, a method of setting the sample decomposition reaction container 10 for microwave heating will be described.

 First, the lower outer cylinder 25 and the upper outer cylinder 24, which are separate bodies, are screwed together and integrated, and the buffer ring 43 is fitted and closely attached to the annular step 26 formed in the upper outer cylinder 24. The buffer ring 43 is an L-shaped ring having a rising portion at the outer edge of the annular ring, and the bottom of the buffer ring 43 abuts the annular step 26, and the outer peripheral surface of the rising portion of the buffer ring 43 is at the top. Abuts the inner peripheral surface of outer cylinder 24. The buffer ring 43 is made of a fluorine-based resin, and is interposed between the outer container 20 and the inner container 30 so that the outer container 20 and the inner container 30 do not directly touch a metal surface or serve as a cushion. It plays a role in enhancing the sealed state of the inner container 30.

 Then, the inner cylinder 33 containing the sample and the solvent is inserted into the outer cylinder 23a. A flange 35 forming a seating surface 34 is formed in an upper part of the inner cylinder 33 to protrude annularly integrally with the inner cylinder 33, and the flange 35 is fitted and fixed to the buffer ring 43. Since the inner diameter of the outer cylinder 23a and the outer diameter of the inner cylinder 33 are the same, the inner cylinder 33 comes into close contact with the outer cylinder 23a.

 Next, the inner lid 31a is seated on the seating surface 34 formed on the upper part of the inner cylinder 33, and the pressing plate 42a is placed on the upper part of the inner lid 31a. The pressing plate 42a is a disk made of stainless steel, and is used for uniformly transmitting the pressing force to the inner lid 31a when the inner container 30 is pressed by the pressing bolt 41a. Thereafter, the outer lid 21a is screwed into the outer cylinder 23a, and the pressure bolt 41a is screwed into the through hole 22 formed in the center of the outer lid 21a. The inner container 30 is pressed by the pressing bolt 41a via the pressing plate 42a, so that the internal sealed state is maintained. Of course, as the pressing means, it is also possible to screw the outer lid 21a, which is not the pressing bolt 41a, to the outer cylinder 23a, and at the same time, press the inner container 30 with the outer lid 21a itself.

The operation of the sample decomposition reaction container for microwave heating 10 according to the present embodiment will be described with reference to FIGS. 2 and 3. Of the reference numerals shown in FIG. 2, reference numeral 50 denotes a microwave generator, reference numeral 51 denotes a housing of the microwave generator 50, reference numeral 52 denotes a microwave irradiation chamber, and reference numeral 53 denotes an openable / closable front surface of the housing 51. The reference numeral 54 indicates the sight glass installed on the door 53. 3, reference numeral 55 denotes a halogen lamp for illuminating the sample decomposition reaction vessel 10 for microwave heating in the microwave generator 50, and reference numeral 60 denotes a slit formed in the outer container 20. Sample and solvent visible through 27a, 27b and inner container 30.

[0026] The sample decomposition reaction vessel 10 for microwave heating in which the sample and the solvent 60 are placed in the inner container 30 is placed on a turntable (not shown) in the microwave irradiation chamber 52. At this time, it goes without saying that the number of the sample decomposition reaction vessels 10 for microwave heating may be plural. The microwave of the microwave generator 50 is oscillated from a magnetron antenna (not shown) and enters the microwave irradiation chamber 52 via a waveguide (not shown), and directly or on the wall of the microwave irradiation chamber 52. Irradiate the microwave heating sample decomposition reaction vessel 10 rotating with the turntable while reflecting. The sample and the solvent 60 are heated by microwave irradiation, and the sample is decomposed and dissolved in the solvent to form a solution. In this case, the sample decomposition reaction vessel 10 for microwave heating is illuminated by a halogen lamp 55 provided in the microwave irradiation chamber 52, and passes through slits 27 a and 27 b formed in the outer vessel 20. Can confirm this process.

 [0027] Note that, even in the case of a plurality of sample decomposition reaction vessels for microwave heating 10, since the sample decomposition reaction vessel for microwave heating 10 rotates together with the turntable, they can be individually confirmed. Also, the process of vertical change of the sample and the solvent 60 in the inner container 30 should be confirmed by the vertical slit 27a drilled in the outer container 20, and the process of horizontal change should be confirmed by the horizontal slit 27b. Can be.

 In the case of a microwave generator without a turntable, the sample decomposition reaction vessel 10 for microwave heating is parallel to the window 54 in order to view it through the window 54. Need to be lined up.

 Example 2

Next, a second embodiment according to the best mode for carrying out the present invention will be described with reference to FIG. 4 or FIG. FIG. 4 is an exploded perspective view of the sample decomposition reaction vessel for microwave heating according to Example 2, FIG. 5 is an assembled cross-sectional view of the sample decomposition reaction vessel for microwave heating according to Example 2, and FIG. 6 is an example. FIG. 4 is an explanatory sectional view for collecting generated gas in an inner container of the sample decomposition reaction container for microwave heating according to 2. 4 to 6, the same elements as those in FIGS. 1 to 3 are denoted by the same reference numerals, description thereof will be omitted, and only different points from the first embodiment will be described.

4 to 6, reference numeral 12 denotes a sample decomposition reaction container for microwave heating according to Example 2, reference numeral 20 denotes an outer container, reference numeral 21b denotes an outer lid of the outer container 20, and reference numeral 22 denotes an outer lid 21b. A through hole formed in the center, reference numeral 23b denotes an outer cylinder of the outer container 20, reference numeral 24 denotes an upper outer cylinder that constitutes the outer cylinder 23b, reference numeral 25 denotes a lower outer cylinder that constitutes the outer cylinder 23b, reference numeral 28 Is a bottom outer cylinder constituting the outer cylinder 23b, reference numeral 30 is an inner container, reference numeral 31b is an inner lid of the inner container 30, reference numeral 33 is a bottomed inner cylinder, reference numeral 41b is a pressure bolt, reference numeral 42b is a pressing plate, Reference numeral 43 denotes a buffer ring, and reference numeral 72 denotes a flow passage opening / closing bolt.

 [0031] In the present embodiment, the outer cylinder 23b of the outer container 20 is composed of an upper outer cylinder 24, a lower outer cylinder 25, and a bottom outer cylinder 28. It is a component. The bottom outer cylinder 28 is screwed to the lower end of the lower outer cylinder 25 and plays a role in improving the stability when the sample decomposition reaction vessel 12 for microwave heating is placed on a laboratory bench or the like. As in the case of 1, even if the bottom outer cylinder 28 is not used as a component, it goes without saying that the effectiveness of the sample decomposition reaction vessel 12 for microwave heating is not affected.

 Also, unlike the first embodiment, a plurality of holes are formed in the outer lid 21b of the outer container 20. This is because the role of the outer container 20 is mainly to prevent the inner container 30 from being deformed when the sample is heated, and the outer container 20 is designed to be lightweight within a range where the deformation preventing function of the inner container 30 is not reduced. is there.

 [0032] The force that the upper surface of the inner lid 31a in Embodiment 1 is flat is 3 lb of the inner lid in this embodiment, and the portion corresponding to the grip of the top is a cylindrical inner lid. Tube 36. A female screw is threaded on the inner peripheral surface of the inner lid tube 36.

The pressure bolt 41b screwed into the through hole 22 formed in the center of the outer lid 21b is a hollow bolt, and the pressure bolt 41b has an inner cap tube penetration hole 73 penetrating therethrough. Is established. And ma When the sample decomposition reaction vessel 12 for the mouth wave heating is set, the inner lid tube 36 is inserted into the inner lid tube penetration hole 73 through the pressing plate 42b, and the top end of the inner lid tube 36 is pressurized with a pressure bolt. It is formed to be almost the same level as the top of 41b.

 [0034] The method for setting the sample decomposition reaction vessel 12 for microwave heating is also substantially the same as the method for setting the sample decomposition reaction vessel 10 for microwave heating.

 That is, the lower outer cylinder 25, the bottom outer cylinder 28, and the upper outer cylinder 24, which are separate bodies, are screwed together and integrated, and the buffer ring 43 is fitted to the annular step portion 26 formed on the upper outer cylinder 24 so as to be closely attached thereto. Let it. Then, when the inner cylinder 33 containing the sample and the solvent is inserted into the outer cylinder 23b, the flange 35 of the inner cylinder 33 is fitted and fixed to the buffer ring 43.

 Next, the inner lid 31b is seated on the seating surface 34 formed on the upper part of the inner cylinder 33, and the pressing plate 42b is placed on the upper part of the inner lid 31b. A hole is formed through the center of the pressing plate 42b, and the inner cover tube 36 projects through the hole. Thereafter, the outer lid 21b is screwed into the outer cylinder 23b, the inner lid 31 is seated on a seating surface 34 formed on the upper part of the inner cylinder 33, and the outer lid 21 is inserted into the insertion hole 22 formed in the center of the outer lid 21. The pressure bolt 41b is screwed in, and the tip of the pressure bolt 41b is brought into contact with the pressing plate 42b. As described above, in this state, the top end of the inner lid tube 36 and the top end of the pressure bolt 41b are substantially the same.

 Then, the flow passage opening / closing bolt 52 is screwed into the inner lid tube 36, and the setting of the microwave heating sample decomposition reaction vessel 12 is completed.

 In this set state, the lower end of the inner container 30 and the upper surface of the bottom outer cylinder 28 are slightly apart. This prevents the lower surface of the inner container 30 from contacting the upper surface of the bottom outer cylinder 28 when the inner container 30 is pressed by the pressure bolt 41, and the inner container 30 expands downward due to heating. Sometimes, the lower end portion of the inner container 30 and the upper surface of the bottom outer cylinder 28 come into contact with each other to prevent the inner container 30 from being further deformed.

Next, the pressing means and the gas discharging means in the present embodiment will be described.

First, the pressing means in the present embodiment will be described. The pressing means in the present embodiment is firstly different from the pressing means in the embodiment. That is, when the pressing bolt 41b is screwed into the through hole 22 of the outer lid 21b and rotated clockwise, the tip of the pressing bolt 41b contacts the pressing plate 42b. Pressing the pressure bolt 41b clockwise further increases the pressure. The tip of the bolt 41b presses the pressing plate 42b so as to push it down. In pressing, since the inner lid tube 36 is slidable with respect to the pressure bolt 41b, the inner lid tube 36 does not hinder the pressing force by the pressure bolt 41b.

Next, the gas discharging means in the present embodiment will be described based on FIGS. 5 and 6. FIGS. 5 and 6 show a state in which the sample decomposition reaction vessel 12 for microwave heating according to the present embodiment is set. FIG. 5 shows a state in which a gas flow path constituting the gas discharge means is shut off, and FIG. 6 shows a state in which a gas flow path constituting the gas discharge means is formed.

5 and 6, reference numeral 37 denotes a conical projection projecting from the lower surface of the inner lid 31b, reference numeral 60 denotes a sample and a solvent, reference numeral 61 denotes a generated gas, and reference numeral 62 denotes a generated gas collector. Reference numeral 74 denotes a gas flow passage opening formed above the flow passage opening / closing bolt 72, reference numeral 75 denotes a first flow passage, reference numeral 77 denotes a second flow passage, and reference numeral 78 denotes a flow passage opening / closing to the inner cover tube penetration hole 73. Reference numeral 79 denotes an annular rib formed below the flow passage opening / closing bolt 72 when the bolt 72 is screwed.

 [0040] A small-diameter hole is drilled along the axis of the flow passage opening / closing bolt 72, and near the lower end of the flow passage opening / closing bolt 72, the hole is bent at a right angle and its tip is opened to the outside. A second flow passage 77 is formed. The other end of the second flow passage 75 is connected to the gas flow passage opening 74. The gas flow passage opening 74 has a cup shape with an open top, and in this embodiment, the diameter of the gas flow passage opening 74 is approximately 4 mm, and the diameter of the second flow passage 77 is approximately 1.5 mm. It is not limited to this numerical value.

The first flow passage 75 is formed by penetrating a small-diameter hole from the inner bottom of the cylindrical inner lid tube 36 of the inner lid 31b to the tip of the conical projection 37. Therefore, when the sample decomposition reaction vessel 12 for microwave heating is set, the lower end of the first flow passage 75 is opened into the inner container 30. In the present embodiment, the diameter of the first flow passage 75 is set to approximately 1.8 mm, but is not limited to this value like the diameter of the second flow passage 77. The conical projection 37 has a root portion slightly larger than the inner diameter of the inner cylinder 33, and the inner lid 31b is seated on a seating surface 34 formed on the upper part of the inner cylinder 33. When the inner cover 31 is placed, the inner cover 31 is seated at a predetermined position without being shifted with respect to the inner cylinder 33, and has a role of bringing the inner cover 31b into close contact with the inner cylinder 33 when the inner cover 31b is pressed. The conical projection 37 is also provided on the lower surface of the inner lid 31a in the first embodiment.

[0042] The flow passage opening / closing bolt 72 has a hexagonal column at the upper part, a male screw threaded at the lower part, and a cylindrical part at the lower part, which is larger than the diameter of the part at which the male screw is threaded. The diameter of the column is smaller. An annular rib 79 is formed at the upper part of the cylindrical portion, and the diameter of the annular rib 76 is formed to be substantially the same as the inner diameter of the cylindrical inner lid tube 36 of the inner lid 31b. ing. The lower end of the second flow passage 77 is open to the outside at the position of the cylindrical portion of the flow passage opening / closing bolt 72 and below the annular rib 79.

 With the sample decomposition reaction container 12 for microwave heating set, the flow passage opening / closing bolt 72 is screwed into the inner lid tube 36, and the lower end of the flow passage opening / closing bolt 72 is applied to the bottom of the inner lid tube 36. After the contact, the flow passage opening / closing bolt 72 is slightly turned to the left, and the bottom of the inner lid tube 36 and the lower end of the flow passage opening / closing bolt 72 are in the state shown in FIG.

 As shown in FIG. 6, since the cylindrical portion of the flow passage opening / closing bolt 72 is smaller than the inner diameter of the inner lid tube 36, the circumference of the cylindrical portion becomes an annular space, and the flow passage space 78 is formed. That is, the flow passage space 78 is closed by an upper portion closed by an annular rib 79, and a lower portion is formed by a space formed by a lower end of the flow passage opening / closing bolt 72 and a bottom portion of the inner lid tube 36.

 By connecting the upper end of the first flow passage 75 and the lower end of the second flow passage 77 to this flow passage space 78, the inside of the inner container 30 and the gas flow passage opening 74 are connected. Communication and gas flow passages are formed.

On the other hand, with the sample decomposition reaction vessel 12 for microwave heating set, the flow passage opening / closing bolt 72 is screwed into the inner lid tube 36, and the lower end of the flow passage opening / closing bolt 72 is inserted into the bottom of the inner lid tube 36. 5, the lower end of the flow passage opening / closing bolt 72 closes the upper end of the first flow passage 75 as shown in FIG. Therefore, the gas flow path is blocked at the upper end of the first flow path 75, and the formation of the gas flow path is hindered. Since both the inner lid 30 and the flow passage opening / closing bolt 72 are made of resilient fluorinated propylene resin, tetrafluorinated styrene resin or perfluoroalkoxy resin, they adhere to each other with a slight force. The method of heating the sample decomposition reaction vessel 12 for microwave heating according to the present embodiment containing the sample is similar to that of the sample decomposition reaction vessel 10 for microwave heating of the first embodiment. Since the process can be performed using 50, the description is omitted, but here, mainly, the handling of the sample decomposition reaction vessel 12 for microwave heating before and after heating by the microwave generator 50, the method, Will be explained.

 When it is desired to add a solvent or the like to the sample decomposition reaction vessel 12 for microwave heating in which the sample and the solvent 60 are accommodated in the inner container 30, by removing the flow passage opening / closing bolt 72, the bottom of the inner lid tube 36 is removed. The upper end of the first flow passage 75 communicating with the inside of the inner container 30 appears. By inserting the needle tip (not shown) of the syringe from the upper end of the first flow passage 75, a desired amount of solvent or the like can be additionally injected, that is, injected.

 After the addition of the solvent, etc., the flow passage opening / closing bolt 72 is screwed into the inner lid tube 36, and the lower end of the flow passage opening / closing bolt 72 contacts the bottom of the inner lid tube 36, and the inner container 30 is sealed. Then, it is placed in a microwave generator 50 and heated.

 [0048] After heating in microwave generator 50 for a predetermined period of time, or through slits 27a and 27b formed in outer container 20, sample can be viewed through window 54 of microwave generator 50. After confirming the state of the solvent 60, the sample decomposition reaction vessel 12 for microwave heating is taken out of the microwave generator 50.

 If the outer lid 21b of the outer container 20 is removed in this state, the reacted sample and the solvent 60 may be ejected from the inner container 30, which is at a high pressure due to the generated gas 61 generated by the reaction between the sample and the solvent 60. is there. In order to avoid such a situation, before removing the outer lid 21b of the outer container 20, turn the flow passage opening / closing bolt 72 counterclockwise to form a gas flow passage connecting the inside of the inner container 30 and the gas flow passage opening 74. Then, the generated gas 61 is released to the outside to make the gas pressure inside the inner container 30 equal to the outside pressure. When the generated gas 61 is toxic, the generated gas 61 can be collected by a generated gas collector 62 as shown in FIG.

 Example 3

 Next, a third embodiment according to the best mode for carrying out the present invention will be described with reference to FIG.

FIG. 7 is an assembled cross-sectional view of a sample decomposition reaction container for microwave heating according to Example 3. In FIG. 7, the same elements as those in FIGS. 1 to 6 are denoted by the same reference numerals and the description thereof will be omitted, and only the differences from the first and second embodiments will be described. .

 In FIG. 7, reference numeral 14 denotes a sample decomposition reaction container for microwave heating according to Example 3, reference numeral 20c denotes an outer container, reference numeral 21c denotes an outer lid constituting the outer container 20c, and reference numeral 22 denotes an outer lid 21. Reference numeral 23c denotes an outer cylinder constituting the outer container 20c, reference numeral 38 denotes a packing body, reference numeral 72 denotes a flow passage opening / closing bolt, and reference numeral 76 denotes a first flow passage.

 [0051] The pressing means in this embodiment is composed of a female screw threaded on the inner peripheral surface of the upper part of the outer cylinder 25c, and a male screw threaded on the outer peripheral surface of the outer lid 21c. That is, the inner cylinder 33 is inserted into the outer cylinder 23c, and the flange 35 of the inner cylinder 33 is fitted to the annular step 26. Then, the outer lid 21c is screwed into the outer cylinder 23c and the upper part of the inner cylinder 33 is inserted. By pressing from inside, the inside of the inner cylinder 33 is made to be in a sealed state.

 [0052] In the present embodiment, the inner lid 31a and the inner lid 31b used in the first and second embodiments are not included as components. Therefore, in order to increase the degree of sealing between the inner cylinder 33 and the outer lid 21c, a ring-shaped packing body 38 is protruded from the lower surface of the outer lid 21c. The packing body 38 is made of a disc-shaped elastic body having a diameter slightly larger than the inner diameter of the inner cylinder 33. When the outer lid 21c is fitted to the inner cylinder 33, the outer peripheral edge of the packing body 38 is formed. The inner cylinder 33 is in close contact with the inner peripheral surface. Therefore, the outer lid 21c is made of a polyimide resin instead of a metal. In this case, the outer cylinder 23c of the outer container 20c is also made of a polyimide resin, so that the sample decomposition reaction vessel for microwave heating 14 according to the present embodiment is the microwave heating sample decomposition reactor 14 according to the first and second embodiments. Considerably lighter than the sample decomposition reaction vessel.

 [0053] In addition, a flow passage opening / closing bolt 72 is screwed into the through hole 22 formed in the center of the outer lid 21c. Then, a small-diameter hole is formed so as to connect the through hole 22 and the lower surface of the outer lid 21c, and a first flow passage 76 is formed.

 Therefore, the outer lid 21c also functions as the pressure bolt 41b and the inner lid 31b in the second embodiment.

Although the pressurizing means in the present embodiment has been described above, the gas discharging means in the present embodiment is the same as the gas discharging means in the second embodiment, and a description thereof will be omitted. Further, the method for heating the sample decomposition reaction vessel for microwave heating 14 according to the present embodiment and the method for handling the sample decomposition reaction vessel for microwave heating 14 before and after heating by the microwave generator 50 are also described in Example 2. Since the heating method and the handling method of the sample decomposition reaction container 14 for microwave heating are the same as those of the first embodiment, the description is omitted.

 As described above, the sample decomposition reaction container for microwave heating 14 according to the present embodiment is a so-called simple type sample decomposition reaction container for microwave heating, and the handling thereof is easy. Heat resistance and pressure resistance are slightly inferior to those of the sample decomposition reaction containers for microwave heating according to Example 1 and Example 2.

Claims

The scope of the claims  [1] an outer container including an outer cylinder provided with a plurality of slits and an outer lid detachably screwed to an upper portion of the outer cylinder;  An inner container having a bottomed translucent inner cylinder or an inner container having a bottomed translucent inner cylinder and an inner lid seated on the upper part of the inner cylinder;  The outer peripheral surface of the inner cylinder is housed in the outer container in close contact with the inner peripheral surface of the outer cylinder, and the inner cylinder and the outer lid are pressed by pressing means, or the inner cylinder and the inner lid are pressed. A sample decomposition reaction container for microwave heating, wherein the container is pressed by means to maintain a sealed state inside the inner container.  [2] The outer cylinder and the outer lid are made of a material made of at least one of stainless steel, alumina sintered body, or polyimide resin, or a combination thereof.  The inner cylinder is a material made of one or a combination of glass, quartz glass, fluorinated ethylene propylene resin or perfluoroalkoxy resin,  The microwave heating sample according to claim 1, wherein the inner lid is made of a material made of one or a combination of a fluorinated propylene resin, a tetrafluoroethylene resin, and a perfluoroalkoxy resin. Decomposition reaction vessel. [3] A gas discharge unit which enables communication between the inside of the inner container and the outside of the outer container in a hermetically sealed state in which the inner container is pressed by the pressing unit. The sample decomposition reaction vessel for microwave heating according to claim 2. [4] The pressing means may be configured to be pressed by screwing the outer lid into the outer cylinder. The gas discharging means may be vertically penetrated at a central portion of the outer lid and penetrated in a vertical direction. 1) and a flow passage opening / closing bolt having a second flow passage penetrating vertically and screwed into the outer lid, and a lower end of the flow passage opening / closing bolt is provided on the outer lid surface. The gas flow passage is shut off by being in close contact with the outer cover surface, and the gas flow passage is formed by separating the lower end of the flow passage opening / closing bolt from the outer lid surface. 4. The sample decomposition reaction container for microwave heating according to claim 3. [5] The pressing means is configured to be pressed by a pressure bolt screwed into a central portion of the outer lid. And  The gas discharging means has a first flow passage penetrating in a vertical direction formed in a central portion of the inner lid, and a second flow passage penetrating in a vertical direction, and has a second flow passage penetrating the outer lid, A flow passage opening / closing bolt screwed into the inner lid, wherein the lower end of the flow passage opening / closing bolt is brought into close contact with the inner lid surface to shut off a gas flow passage. 4. The sample decomposition reaction vessel for microwave heating according to claim 1, wherein a gas flow passage is formed by being separated from the inner lid surface. [6] An annular step is formed inside the upper part of the outer cylinder,  6. The microwave heating device according to claim 1, wherein a flange formed at an upper portion of the inner cylinder is fitted to the step, and the inner container is fixed to the outer container. Sample decomposition reaction vessel.  [7] The outer cylinder comprises an upper outer cylinder having an annular step formed therein and a lower outer cylinder having a plurality of slits formed therein.  7. The sample decomposition reaction container for microwave heating according to claim 1, wherein the upper outer cylinder and the lower outer cylinder are detachably screwed to each other.