JP3035549B1 - Powder sample filling device for sealed sample containers - Google Patents

Abstract

Abstract: PROBLEM TO BE SOLVED: To prevent a powder sample from adhering to a seal portion of a sample container main body at the time of filling a powder sample into a sealed small sample container, thereby preventing measurement failure due to poor sealing or damage to a thermal analyzer. And workability in the glove box can be greatly improved. SOLUTION: A sample container holder 12 for holding a sample container main body 12, a funnel 22 for supplying a powder sample located above an opening of the sample container main body, a funnel holding unit 24, a funnel elevating mechanism 26, and a funnel elevating / lowering The apparatus includes a lifting / lowering amount measuring device (dial gauge 28) for measuring the amount, a pushing rod 30 that can be inserted into the thin tube portion of the funnel, and a rod guide portion 32 that guides the pushing rod up and down. The lower end of the thin tube portion of the funnel is inserted below the seal portion in the sample container main body, and the powder sample supplied to the expanded portion of the funnel is filled into the sample container main body by the vertical movement of the pushing rod.

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to an apparatus for filling a sealed sample container with a powder sample by using a funnel and a push rod which moves up and down so that the powder sample does not adhere to a seal portion of the container. is there. This apparatus is suitable for producing a small sample for thermal analysis in a glove box, for example.

[0002]

2. Description of the Related Art When measuring the thermal characteristics of a powder sample having a high chemical activity (such as a Na compound) with a thermal analyzer, a sealed small sample container (for example, an external device) for thermal analysis is used in a glove box in an inert gas atmosphere. It is necessary to fill and enclose a powder sample in a diameter of 5 mm and a height of 5.4 mm).

As shown in FIG. 4A, a sample container 10
Sample container main body 12 and lid 14 for closing the upper opening
And a combination of As shown in FIG. 4B, after filling a predetermined amount of the powder sample 16 into the sample container body 12,
The lid 14 is fitted, and the upper edge 1 of the sample container body 12 is opened.
Seal 2a by swaging. Here, the opening diameter D of the sample container main body 12 is as small as about 3 mm.

Conventionally, as shown in FIG. 5, a predetermined amount of a powder sample 16 is placed on a folded medicine package paper 18, and the powder sample 16 is held by a hand (in a glove box operation, by a hand wearing a glove). The powder sample 16 was filled in the sample container body 12 by pouring from the opening.

[0005]

However, as described above, the sample container is very small and the opening thereof is very narrow, and the workability is poor due to the work in the glove box. As shown in FIG. 6, the powder sample 16 adheres to the seal portion 12b between the lid 14 and the inner wall of the opening of the sample container main body 12, so that a gap is generated between the sample container main body 12 and the lid 14. In some cases, sealing failure occurred. If the sample container 10 is not completely sealed, the sample may be deteriorated during the thermal analysis test and the measurement may fail. If it is severe, the sample may be ejected due to an increase in the internal pressure of the sample container during the test, or the thermal analyzer may be used. May be damaged.

Therefore, it is possible to prevent the powder sample from adhering to the sealing portion 12b between the inner wall of the opening of the sample container main body 12 and the lid 14, and to facilitate the sample filling operation in the glove box. However, this was a major problem in performing thermal analysis efficiently and accurately.

An object of the present invention is to prevent a powder sample from adhering to a seal portion of a sample container body at the time of filling a powder sample into a sealed small sample container, thereby failing in measurement due to defective sealing or a thermal analysis apparatus. An object of the present invention is to provide a device which can prevent breakage and can greatly improve workability in a glove box.

[0008]

According to the present invention, there is provided a sample container holder for holding a sample container main body, a funnel for supplying a powder sample located above an opening of the sample container main body, and a funnel holding section for holding the funnel. A funnel elevating mechanism for elevating and lowering the funnel holding unit, an elevating amount measuring device for measuring the elevating amount, a pushing rod that can be inserted into the thin tube portion of the funnel from above the funnel,
This is a powder sample filling apparatus for a hermetically sealed sample container having a rod guide section for guiding the rod up and down. The lower end of the thin tube portion of the funnel is inserted below the seal portion in the sample container main body, and the powder sample supplied to the expanded portion of the funnel is filled into the sample container main body by the vertical movement of the pushing rod.

It is desirable that the pushing rod and the rod guide are swingably supported so as to be off the central axis of the funnel. Thereby, the work of attaching and detaching the funnel or the work of supplying the powder sample to the funnel can be easily performed. The funnel elevating mechanism is a mechanism that elevates the funnel holding unit by rotating a ball screw by operating a handle, for example. A dial gauge can be used as the lifting amount measuring device.

[0010] For example, the sample container holder is a combination of a container table and a transparent container holder mounted on the table. The container base has a convex portion in the upper center, and a receiving hole is provided in the convex portion for dropping and housing the lower half of the sample container main body, and the container holder is fitted to the convex portion in the lower center. It has a concave portion for accommodating the upper half of the sample container main body, and has a through hole communicating with the concave portion.

[0011]

FIG. 1 is a schematic view showing an embodiment of an apparatus for filling a powder sample into a hermetically sealed sample container according to the present invention. The powder sample filling apparatus includes a sample container holder that holds the sample container main body 12, a funnel 22 for supplying a powder sample positioned above the opening of the sample container main body 12, and a funnel holding unit 24 that holds the funnel 22. A funnel elevating mechanism 26 for elevating and lowering the funnel holding unit 24, an elevating and lowering amount measuring device (here, a dial gauge 28) for measuring the elevating amount, and a funnel 22 can be inserted into the thin tube portion 22a of the funnel from above the funnel 22. Push rod 30
And a rod guide portion 32 for guiding the vertical movement of the pushing rod. These are all assembled on a single base member 34, so that they can be easily installed in a glove box by being miniaturized and integrated.

The sample container holder 20 holding the sample container main body 12 can be directly mounted on a predetermined position on the base member 34. The powder sample container used here has exactly the same dimensions and structure as those conventionally used as shown in FIG.

FIG. 2 shows the details of the sample container holder. A is a partially cutaway assembly view, and B is a longitudinal sectional view. The sample container holder 20 is composed of a combination of a container table 40 and a container holder 42 placed thereon. Here, both are made of a transparent acrylic resin so that the sample container body 12 housed inside can be observed from the outside. The container table 40 has a circular convex portion 40b at the upper center of a central disk-shaped table main body 40a, and the sample container main body 12
A circular receiving hole 40c for receiving the lower half of the lower part is provided, and a circular convex part 40d is further provided at the center of the lower part. The container retainer 42 has a circular concave portion 42a at the lower center thereof which is fitted to the convex portion 40b and accommodates the upper half of the sample container main body 12, and has a circular through hole 42b communicating with the concave portion 42a. is there.

The lower half of the sample container main body 12 is dropped into the receiving hole 40c at the upper part of the container base 40, and the upper half of the sample container main body 12 is accommodated by covering the container holder 42. Then, the concave portion 42a of the container holder 42 is fitted into the upper central convex portion 40b of the container base 40, and the container holder 42 is integrated with the sample container main body 12 therein. On the other hand, as shown in FIG. 1, a concave portion 44 is formed on the upper surface of the base member 34, and a circular convex portion 40 d on the lower surface of the container base 40 is fitted into the concave portion 44, and The base member 34 and the sample container holder 20, and thus the sample container main body 12 are positioned by pressing the screw 46 in one direction in a plane.

As described above, the sample container holder 20 is used to easily handle the sample container main body 12 which is difficult to handle in the glove box because of its small size. It functions to hold accurately at a predetermined position above.

The funnel 22 for supplying the powder sample is held by a funnel holding part 24 above the opening of the sample container main body 12, and the funnel holding part 24 is moved up and down by a funnel elevating mechanism 26. The funnel 22 is made of glass here, and has a shape that matches the shape of the opening of the sample container main body 12. That is, the outer diameter of the thin tube portion 22 a is designed to be slightly smaller than the opening diameter of the sample container main body 12. The funnel 22 inserts the thin tube portion 22a into the sample container body 12 through the opening when filling the sample container main body 12 with the powder sample, and passes the powder sample supplied to the upper expanding portion 22b through the thin tube portion 22a.
It functions to prevent the powder sample from adhering to the seal portion 12b (see FIG. 4A) of the sample container body 12.

The funnel elevating mechanism 26 has the following structure. An upper fixing plate 52 and a lower fixing plate 54 are attached to the upper end and lower part of one or more main columns 50 erected on the base member 34, respectively. The intermediate portion of the main pillar 50 is fitted to the slide bush 56, and the slide plate 58 incorporating the slide bush 56 is attached to the main pillar 5.
It is slidably provided in parallel along 0. The ball screws 64 are rotatably supported by the bearing units 60 and 62 assembled to the upper fixed plate 52 and the lower fixed plate 54, respectively.
8 and the ball screw nut 66 assembled to the ball screw 6
4 and screwed together. Then, a handle 68 for elevating operation is connected to the upper end of the ball screw 64.

The funnel holder 24 is attached to the slide plate 58. The funnel holding part 24 is provided with the expanding part 22 of the funnel 22.
b, a cylindrical support member 70 into which the lower portion of the thin tube portion 22a is fitted, a connection plate 72 vertically suspended from the support member 70, and a guide member 74 attached to the lower end of the connection plate 72. Become. The guide member 74 has a structure having a guide hole into which the thin tube portion 22a of the funnel 22 just fits. Such a funnel holding portion 24 supports the entire funnel with the support member 70 and the thin tube portion 2 with the guide member 74.
By regulating the tip side of 2a, accurate positioning in the horizontal direction is realized, and the funnel 22 has a function of being held at a predetermined position with respect to the sample container body 12.

The funnel elevating mechanism 26 is a mechanism for inserting the distal end of the thin tube portion 22a of the funnel 22 into the sample container main body 12 and moving it up and down so that the distal end position can be adjusted. When the handle 68 is turned, the ball screw 64 rotates,
The slide plate 58 having the ball screw nut 66 screwed thereto moves up and down in parallel, and the funnel 22 moves up and down.

The vertical movement measuring device is for measuring the vertical movement. Here, a dial gauge 28 is used as a lifting amount measuring device. The dial gauge 28 is mounted on the slide plate 58 and its measuring terminal 28a
Is lowered, and the tip is brought into contact with the upper surface of the lower fixing plate 54. When the slide plate 58 moves up and down, the measuring terminal 28a expands and contracts accordingly, and the amount of movement (the vertical position of the funnel 22) can be read on the scale.

The pushing rod 30 is connected to the funnel 22 made of glass.
Is a stainless steel rod slightly thinner than the inner diameter of the narrow tube portion. The powder sample supplied to the enlarged portion 22b of the funnel 22 using the pushing rod 30 is filled into the sample container body 12 through the narrow tube portion 22a. I do. Accordingly, the push rod 30 is located above the funnel 22. The rod guide portion 32 includes a support 74 erected from the slide plate 58.
And a rod guide plate 76 pivotally attached to the support column 74 and capable of swinging in a horizontal plane, and a rod guide 78 attached to the rod guide plate 76. The rod guide 32 has a guide hole having a diameter slightly larger than the push rod diameter, and the push rod 30 is inserted into the guide hole. The rod guide 78 is configured to be positioned on the center line of the funnel 22 during the powder sample filling operation. The rod guide portion 32 has a function of guiding the push rod 30 to be able to move up and down at a predetermined position. The reason why such a pushing rod 30 is used is that since the sample is powder, it is difficult for the sample to fall naturally only by being put into the funnel 22 made of glass. In addition, since the rod guide plate 76 is swingable, when the funnel 22 is attached to and detached from the funnel holding unit 24 or when the powder sample is supplied to the funnel 22, the funnel 22 escapes from the center line of the funnel, thereby improving workability. Can be improved.

A large-diameter knob portion 80 is fixed to the upper end of the pushing rod 30 to make it easier to pick up when the rod is moved up and down.
Further, a movable stopper 82 is provided at an intermediate portion of the pushing rod 30. In this case, a screw is screwed into the cylindrical member from the side so that it can be fixed to the pushing rod 30 at an arbitrary position. The push rod 30 is provided with a movable stopper 82.
Cannot be lowered below the upper surface position of the rod guide 78, so that when the funnel is detached or the powder sample is supplied, the push rod 30 is obstructed when the rod guide plate 76 is displaced from the center axis of the funnel. Not convenient.

The method of using the device is as follows. The sample container main body 12 is incorporated into the sample container holder 20 and installed on the base member 34. Then, as shown in FIG. 3, the thin tube portion 22a of the funnel 22 is inserted into the sample container body 12. At this time, the thin tube portion 22a is inserted until the distal end thereof is lower than the seal portion 12b of the sample container body 12. In this state, the powder sample is put into the expanding portion 22b of the funnel 22, the pushing rod 30 is lowered from above, and the powder sample 16 is dropped by moving up and down. The powder sample is stored in the thin tube section 2 of the funnel 22.
Although it is difficult to drop naturally by forming a bridge in 2a, the bridge is broken by moving the pushing rod 30 up and down, and flows into the sample container body smoothly because it is fluidized. In this way, the powder sample can be filled in the sample container main body without adhering to the seal portion.

Although the preferred embodiment of the present invention has been described in detail, the present invention is not limited only to such a structure. For example, the funnel elevating mechanism attaches a fixing screw having a leading end to the main column to the slide plate, loosens the fixing screw, moves the slide plate up and down, tightens the fixing screw at an arbitrary position, and moves the slide plate to the main column. It may be configured to be fixed to Further, the elevation measurement device may be a scale plate or the like from which the position of the slide plate can be directly read. The material of the funnel and the push rod is arbitrary, and is not limited to glass or stainless steel. Further, their shapes may be appropriately changed according to the shape of the sample container body.

[0025]

As described above, the present invention is an apparatus for filling a powder sample into a sealed sample container using a funnel and a push rod that moves up and down, so that the powder sample can be transferred to a sealed small sample container in a short time. Can be easily filled. By the way, in the conventional method, the filling operation required about 5 minutes, but by using this apparatus, the operation time could be reduced to about 1/2 to 1/3. In addition, during the powder sample filling operation, the powder sample does not adhere to the seal portion of the sample container body, which can prevent poor sealing at the time of sealing the sample container, and failure of the calorimetric measurement due to the poor sealing. And thermal analysis equipment breakage is drastically reduced. In particular,
Workability in the glove box is significantly improved, and improvement in work quality can be achieved.

The device of the present invention has a simple structure, can be manufactured at low cost, is easy to handle and maintain, and can be miniaturized, so that it is most suitable for work in a glove box.

[Brief description of the drawings]

FIG. 1 is a schematic view showing an embodiment of an apparatus for filling a sample container into a sealed sample container according to the present invention.

FIG. 2 is an explanatory view of the sample container holder.

FIG. 3 is an explanatory diagram showing a supply state of a powder sample according to the present invention.

FIG. 4 is an explanatory view showing an example of a sealed sample container.

FIG. 5 is an explanatory diagram showing a conventional powder sample supply state.

FIG. 6 is an explanatory diagram showing a state of defective sealing in a sealed sample container.

[Explanation of symbols]

 12 Sample container main body 20 Sample container holder 22 Funnel 24 Funnel holding part 26 Funnel elevating mechanism 28 Dial gauge 30 Push rod 32 Rod guide part

──────────────────────────────────────────────────続 き Continued on the front page (58) Field surveyed (Int. Cl. ⁷ , DB name) B65B 1/00-3/36 G01N 1/00 101

Claims (4)

(57) [Claims] 1. A sample container holder for holding a sample container main body, a funnel for supplying a powder sample positioned above an opening of the sample container main body, a funnel holding portion for holding the funnel, and a raising and lowering of the funnel holding portion. A funnel elevating mechanism, an elevating amount measuring device for measuring the elevating amount, a push rod that can be inserted into the thin tube portion of the funnel from above the funnel, and a rod guide portion that guides the vertical movement of the push rod, The lower end of the thin tube portion of the funnel is inserted below the seal portion in the sample container main body, and the powder sample supplied to the expanded portion of the funnel is filled in the sample container main body by the vertical movement of the pushing rod. A powder sample filling device for a sealed sample container. 2. The apparatus for filling a powder sample into a hermetically sealed sample container according to claim 1, wherein the pushing rod and the rod guide are swingably supported so as to deviate from the center axis of the funnel. 3. The sealed sample container according to claim 1, wherein the funnel elevating mechanism is a mechanism for elevating the funnel holding unit by rotating a ball screw by operating a handle, and the elevating amount measuring device is a dial gauge. Powder sample filling equipment. 4. The sample container holder comprises a combination of a container table and a transparent container holder mounted thereon,
The container base has a convex portion at the upper center, and a receiving hole is provided in the convex portion for dropping and storing the lower half of the sample container main body, and the container retainer is fitted to the convex portion at the lower center. 2. A structure having a recess for accommodating the upper half of the sample container body and having a through hole communicating with the recess.
4. A device for filling a powder sample into a sealed sample container according to any one of claims 1 to 3.