JP2008058034A - Container for microwave irradiation - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To perform quickly a large quantity of extremely-low concentration analysis by combining a disposable internal container with an external container having resistance to a microwave. <P>SOLUTION: The analysis container for microwave irradiation has: a constitution including the bottomed disposable internal container 1 comprising a material wherein contamination of a heavy metal is controlled, and having an opening 1a on the upper part; the external container for storing the internal container 1, comprising a non-conductive and heat-resistant material, and having an opening 2a on the upper part; and a sealing member 3 for rupture prevention fitted to the internal and external containers 1, 2. The sealing member 3 for rupture prevention is constituted of: an inner lid 5 having a hole 5a, to be fitted to the opening 1a of the internal container 1; a film 6 comprising a material capable of being ruptured by a pressure; a lid member 7 having a through hole 7a; and an outer lid 8 for pressure-contacting the lid member 7 with the opening 1a of the internal container 1. <P>COPYRIGHT: (C)2008,JPO&INPIT

Description

  The present invention relates to a container for microwave irradiation, and more particularly to a container for microwave irradiation that is capable of extremely low concentration analysis and is suitable for rapidly processing a large amount of sample.

Due to the recent increase in environmental and health awareness, detection of extremely low concentrations of ppb to ppt is required in the analysis of soil and food, and a large amount of samples must be processed quickly.
In such low-concentration analysis, the use of disposable instruments managed at a strict level for trace analysis is generally performed because analysis instruments, contamination in the cleaning process, etc. interfere with the analysis.
As an instrument used for such an application, for example, DigiTUBE (manufactured by SCP Science) made of metal-free polypropylene is known (for example, Non-Patent Document 1).

On the other hand, when it is desired to irradiate microwaves in the course of analysis, sample pretreatment, etc., the polypropylene container is deformed and damaged, and cannot be used as it is.
Therefore, for such applications, for example, “Microwave Vessel Nano-Band MV Series” (GL Sciences Inc.) is provided (for example, Non-Patent Document 2).

  This container is manufactured as a closed type decomposition container that realizes microwave thermal decomposition of a solid sample using a microwave oven. When analyzing using this container, first, a sealed container made of fluororesin is used. Inside, an internal small container made of fluororesin is installed, and a solid sample such as soil is put into the internal small container.

SCP Science website, DigiTUBE catalog, [Search August 23, 2006], Internet <http://www.scpscience.com/products/Digestion/digitubes.asp> GL Sciences Inc., Nano-Band MV series catalog, [Search August 23, 2006], Internet <http://www.gls.co.jp/product/catalog-28/02/26.html>

However, this small inner container is not disposable and needs to be washed and used every time. The washing is complicated and not suitable for processing a large amount of sample. Moreover, there is a problem that contamination may occur due to the cleaning process, and accurate measurement is difficult due to this contamination.
The present invention combines a disposable internal container that contains a sample and an external container that is resistant to microwaves, so that it is possible to perform extremely low concentration analysis and to process a large number of samples quickly. An object is to provide an analysis container for wave irradiation.

The analysis container for microwave irradiation according to the present invention is formed of a material in which mixing of heavy metals is controlled, and has a bottomed disposable inner container having an opening at the top,
An outer container that is formed of a non-conductive and heat-resistant material, has an opening at the top, and houses the inner container;
A burst preventing seal member fitted to the inner container and the outer container,
The rupture prevention seal member has an inner lid that has a hole and is fitted to the opening of the inner container, a film formed of a material that can be ruptured by pressure, a lid member that has a through hole, and the lid member And an outer lid for press-contacting with the opening of the inner container.

In this analysis container for microwave irradiation, the inner container is preferably formed of polyolefin or polystyrene.
The outer container preferably has a hole at the bottom that is smaller than the outer diameter of the inner container, and further preferably includes a movable bottom member that can close the hole of the outer container.
When the rupture prevention seal member is fitted to the inner container and the outer container, the hole of the inner lid communicates with one end of the through hole of the lid member through the film, and the other end of the through hole of the lid member is The hole and the through hole are preferably formed so as to communicate with the outside.
The inner lid may have a groove fitted to the opening of the inner container on the inner periphery thereof.

  According to the container for microwave irradiation of the present invention, by combining a disposable internal container for storing a sample and an external container imparted with resistance to microwaves, there is no problem of contamination resulting from complicated operations such as cleaning. In addition, ultra-low concentration analysis using a contamination-free disposable container can be performed more accurately and quickly on a large number of samples.

As shown in FIG. 1, the analysis container for microwave irradiation according to the present invention mainly includes an inner container 1, an outer container 2, a burst preventing seal member 3, and optionally a movable bottom member 4. Is done.
This analytical container for microwave irradiation can be suitably used for microanalysis, in particular, measurement of elution concentration of heavy metal by acid, and is used only once for a portion that directly contacts the sample (that is, internal container, etc.) It is intended to be disposable.

The inner container is inexpensive, suitable for disposable use, and is a material that can be easily mixed with heavy metals, and the heavy metal content is controlled (preferably, the heavy metal content is controlled to the ppt level (about 10 ^-12 g / cm ³ ) or less. It is preferable that it is made of a material made of Specific examples include polyolefins such as polyethylene (PE) and polypropylene (PP), polystyrene (PS), and the like. Of these, polyolefins such as PP are particularly preferred because of their good processability.

The shape and size of the inner container are not particularly limited, but it is preferably a shape and size suitable for microanalysis. For example, a commercially available metal-free container such as DigiTUBE described above can be used as it is. In addition, although the lid | cover is usually attached to the commercially available container, it is preferable to use in the state which removed such a lid | cover in the microwave irradiation container of this invention.
Specifically, the shape of the inner container is suitably a cylindrical shape having an opening in the upper portion, a bottomed cylindrical shape, an elliptical cylindrical shape, a rectangular cylindrical shape, or a cylinder similar thereto. Of these, a cylindrical shape is preferable.

The outer container is not necessarily intended to be disposable, and in order to prevent deformation and breakage of the inner container when microwave irradiation is performed directly on the inner container, the inner container can be accommodated therein, What is necessary is just to be formed with the material which is nonelectroconductive and has heat resistance. By having such characteristics, it is possible to sufficiently withstand the microwave irradiation to the object accommodated in the inner container. Here, non-conductive refers to, for example, one having an internal resistance of about 10 ⁻⁵ Ωm or more. Moreover, heat resistance means that the excessive deflection temperature (thermal deformation temperature) at 0.45 Mpa defined in JIS K7191 “Plastics—Test method for deflection temperature under load” is 130 ° C. or higher.

  Various resins are listed as satisfying these characteristics. Specifically, fluororesin (for example, PTFE: polytetrafluoroethylene, PFA: tetrafluoroethylene / perfluoroalkyl vinyl ether copolymer, FEP: tetrafluoroethylene / hexafluoropropylene copolymer, ETFE: tetrafluoroethylene / Ethylene copolymer, PVDF: polyvinylidene fluoride, PCTFE: polychlorotrifluoroethylene, ECTFE: chlorotrifluoroethylene / ethylene copolymer, etc.), polyacetal copolymer, nylon, polycarbonate, polyetherketone, polyimide, polyether Examples include imide, polyether sulfone, polyphenylene sulfide, and phenol resin. In particular, a fluororesin, a polyacetal copolymer and the like are suitable. In the present invention, since the outer container does not directly touch the sample, the degree of freedom of the material used for this portion is higher than that of the inner container.

The external container can ensure pressure resistance by appropriately adjusting the material, thickness, and shape thereof. For example, it has an opening for inserting the inner container in the upper part, and a male screw or a female screw is formed on the upper outer peripheral surface of the outer container so as to be screwed with the inner peripheral surface of the outer lid described later. It is preferable. Thereby, the inner container can be reliably sealed by the outer container and the outer lid.
Moreover, it is preferable that an outer container has a hole smaller than the outer diameter of an inner container in the bottom part. One hole may be provided, but a plurality of holes may be formed. By using this hole together with the movable bottom member described later, the inner container can be easily taken out.

  The rupture prevention seal member is fitted to the inner container and the outer container, respectively, and seals the inside of the inner container, and has a function of releasing the expanded gas when the contents of the inner container are expanded by microwave irradiation or the like. And includes a plurality of independent members, that is, an inner lid, a film, a lid member, and an outer lid.

The inner lid is formed to be slightly larger than the outer diameter of the inner container in order to fit into the opening of the inner container, and has a hole penetrating from the surface (the outer lid 8 side in FIG. 1) to the back surface. . One hole may be provided, but a plurality of holes may be formed. The size of the hole is appropriately adjusted according to the size of the inner container, the type of the object to be measured, and the like, for example, about 1 to 3 mm ² is appropriate.
The shape of the inner lid may be a plate-like body, or may be a shape in which the peripheral portion of the front surface and / or the back surface protrudes (see FIG. 1). By providing the inner lid, a film to be described later can be held between the surfaces, and the airtightness of the inner container can be ensured.

Further, by forming protrusions on the peripheral edge of the surface, it becomes easy to dispose a film to be described later in the protrusions (see FIG. 2), and it is possible to prevent the film from shifting.
Furthermore, it is preferable that a surface that fits into the opening of the inner container is provided with a groove that fits the opening of the inner container in the vicinity of the peripheral edge thereof. Thereby, airtightness can be raised more with the raise of the internal pressure of an inner container.
The protruding shape described above may be formed in combination with a groove.

  The film is a material that can be ruptured by pressure, and is usually preferably a material that does not allow gas and liquid to pass through. The pressure which can be destroyed in this case is, for example, about 0.5 to 10 MPa. As the film material, for example, various materials such as polyolefin such as PE and PP, vinyl chloride resin, silicon resin and the like can be used. By using such a material, when the object in the inner container is irradiated with microwaves, the gas in the inner container, the object to be measured, etc. expands and becomes extremely pressurized. Thus, the internal pressure can be released. Moreover, since it is a material which does not allow a base | substrate and a liquid to pass through normally, the airtightness of an inner container can be ensured in the state without an extreme pressure load.

  The shape and size of the film are not particularly limited, but it is necessary that the film has a shape and size capable of completely closing at least the hole of the inner lid described above. Moreover, it is preferable that it is substantially the same as the shape and magnitude | size of an inner cover, or smaller than it. As a result, the film can be firmly sandwiched between the inner lid and the lid member described later, the airtightness of the inner container can be secured, and the film can be easily ruptured by concentrating the pressure when pressure is applied. be able to.

  The lid member mainly plays a role of sandwiching the above-described film (preferably by a surface) and transmitting a pressure contact force by an outer lid described later to the film and the inner lid. The shape of the lid member is not particularly limited, and may be, for example, a circular, elliptical, polygonal, or a planar columnar shape similar to these, but a protrusion is provided at the center of these planar plate-like bodies. The shape is preferred. The size is not particularly limited, but on the side in contact with the film, it must be at least large enough to hold the film, slightly larger than the outer diameter of the inner container and substantially the same as the inner lid Alternatively, it is preferably slightly larger and / or substantially the same as or slightly larger than the film. In addition, the back surface of the lid member may be flat (see FIG. 1) or may have a shape in which the peripheral edge protrudes. By forming the protrusions on the peripheral edge, it becomes easy to dispose the film in the protrusions, and displacement of the film can be prevented. Moreover, it becomes easy to fix the protrusion formed on the peripheral edge to the inner lid by fitting the protrusion on the outer periphery or the inner periphery of the protrusion formed on the surface.

  A through hole is formed in the lid member. The through-hole may be linearly penetrated from the upper surface to the lower surface, but is preferably bent in the lid member two-dimensionally or three-dimensionally. Because the through-hole is bent in this way, when the film is ruptured due to pressure, the contents of the container come into contact with the upper part of the irradiation chamber in a microwave irradiator that usually has an irradiating device disposed on the upper surface. Can be prevented.

  Moreover, it is preferable that this through-hole is the same size as the hole of the inner cover mentioned above, or is somewhat large, for example. Further, when the burst preventing seal member is fitted to the inner container and the outer container, one end of the through hole is formed on the back surface of the lid member so as to communicate with the hole of the inner lid via the film. It is preferable that the through hole is formed so that the other end communicates with the outside. In particular, when the lid member has a shape including a protrusion at the center of the plate-like body, one end of the through hole is arranged near the center of the plate-like body, and the other end of the through hole is arranged on the side surface of the protrusion. It is preferable that By adopting such a shape, it is easy to transmit a pressure contact force by an outer lid, which will be described later, to the film and the inner lid, and gas from the inner container can be easily released through the through hole.

  The outer lid presses the lid member, and further, the film and the inner lid against the opening of the inner container to seal the inner container and protect the inner container from direct microwave irradiation. The shape of the outer lid is not particularly limited, but it is preferable that one end is opened and the other end is bottomed, and the outer lid has a cylindrical shape corresponding to the outer shape of the outer container. In particular, it is preferable that the outer periphery of the cylindrical container is formed with a male screw or a female screw to be screwed with the upper outer peripheral surface of the outer container.

Moreover, it is preferable that a hole is formed in the upper surface of the outer lid. The hole preferably has a size and shape that exposes or protrudes a part of the surface of the lid member, preferably a part of the protrusion. With this hole, the other end of the through hole formed in the lid member can be guided to the outside.
The inner lid, the lid member, and the outer lid described above can be formed of the materials exemplified for the outer container. In particular, since the inner lid and the film may contact or rupture the object to be measured, the inner lid and the film can be formed of a material that is inexpensive and suitable for disposable use.

  When the analysis container for microwave irradiation of the present invention has a hole in the bottom of the external container, it is preferable to arbitrarily include a movable bottom member. The movable member is preferably larger than the hole at the bottom of the outer container and is substantially the same as or slightly smaller than the inner diameter of the bottom of the inner container. By having this movable bottom member, the inner container can be easily removed by moving the movable bottom member in the direction of arrow A in FIG. 2 through the hole in the bottom.

Below, the Example of the analytical container for microwave irradiation of this invention is shown in detail based on drawing.
Example 1
As shown in FIGS. 1 and 2, the analysis container for microwave irradiation of this example has, as an inner container 1, a commercially available DigiTUBE made of PP, an outer container 2 made of Duracon (polyacetal copolymer), and a rupture. The prevention seal member 3 includes an inner lid 5 made of PTFE, a film 6 made of PE, a lid member 7 made of PTFE, an outer lid 8 made of Duracon, and a movable bottom member 4 made of Duracon.
In this analysis container for microwave irradiation, the opening of DigiTUBE which is the inner container 1 has a diameter of 30 mm and a volume of 50 cc. The hole 5a of the inner lid 5 has a diameter of 2 mm. The thickness of the film 6 is 0.03 mm. The through hole 7a of the lid member 7 was 3 mm in diameter.

Thus, by using the analysis container for microwave irradiation according to the present invention, the airtightness of the object to be measured in the inner container can be secured by the film, and the external container itself is expelled when irradiated with microwaves. Can be prevented.
Further, by using the movable bottom member, the inner container that is in close contact with the outer container can be easily taken out.
Furthermore, since the inner container is a disposable container, it is possible to quickly analyze a large number of samples without performing complicated operations such as washing and without contamination by impurities.

Example 2
As shown in FIG. 3A, the analysis container for microwave irradiation of this example has a shape in which a peripheral part protrudes by forming a recessed part 7 b in the center part of the back surface of the lid member 7. Except for this, the configuration is substantially the same as the microwave irradiation analysis container of Example 1.
As described above, since the concave portion is formed on the back surface of the lid member, the film can be more firmly sandwiched and the hermeticity of the inner container can be ensured.

Example 3
As shown in FIG. 3B, the analysis container for microwave irradiation of this embodiment has a groove formed in the vicinity of the outer periphery on the back surface of the inner lid 5, and a recess formed in the central portion so as to be connected to the groove. By forming 5d, the configuration is substantially the same as the analysis container for microwave irradiation of Example 1 except that the peripheral edge protrudes.
As described above, since the recess is formed on the back surface of the inner lid, the film can be more firmly sandwiched, and the hermeticity of the inner container can be ensured.

  The analysis container for microwave irradiation according to the present invention can be preferably used for all analyzes in which microwave irradiation is performed regardless of the presence or absence of microwave irradiation.

It is an exploded view which shows the analytical container for microwave irradiation in one Embodiment of this invention. FIG. 2 is an assembled cross-sectional view of the microwave irradiation analysis container of FIG. 1. It is a partial exploded view which shows the analytical container for microwave irradiation in another embodiment of this invention.

Explanation of symbols

DESCRIPTION OF SYMBOLS 1 Inner container 1a, 2a Opening 2 Outer container 2b, 5a, 8a Hole 3 Burst prevention sealing member 4 Movable bottom member 5 Inner lid 5b Groove 5c, 5d Recess 6 Film 7 Lid member 7a Through hole 8 Outer lid

Claims (6)

A disposable inner container with a bottom formed by a material in which the mixing of heavy metals is controlled and having an opening in the upper part;
An outer container that is formed of a non-conductive and heat-resistant material, has an opening at the top, and houses the inner container;
A burst preventing seal member fitted to the inner container and the outer container,
The rupture prevention seal member has an inner lid that has a hole and is fitted to the opening of the inner container, a film formed of a material that can be ruptured by pressure, a lid member that has a through hole, and the lid member An analysis container for microwave irradiation, comprising: an outer lid for press-contacting the container to the opening of the inner container.   The analysis container for microwave irradiation according to claim 1, wherein the inner container is formed of polyolefin or polystyrene.   The analysis container for microwave irradiation according to claim 1 or 2, wherein the outer container has a hole at its bottom that is smaller than the outer diameter of the inner container.   Furthermore, the analytical container for microwave irradiation of Claim 3 provided with the movable bottom member which can close the hole of an external container.   When the rupture prevention seal member is fitted to the inner container and the outer container, the hole of the inner lid communicates with one end of the through hole of the lid member through the film, and the other end of the through hole of the lid member is The analysis container for microwave irradiation according to any one of claims 1 to 4, wherein the hole and the through hole are formed so as to communicate with the outside.   The analysis container for microwave irradiation according to any one of claims 1 to 5, wherein the inner lid has a groove fitted to the opening of the inner container on an inner periphery thereof.

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