JP2571706B2 - Crimper for sealing cell mouth - Google Patents

Description

DETAILED DESCRIPTION OF THE INVENTION [Industrial application field] At present, many chemical substances are used in various places, but it is necessary to know the danger of these chemical substances and to handle them accordingly. Given the magnitude of the disaster that chemicals can cause, it is a duty imposed on users.

The present invention, among these dangers, fire, explosion danger thermal properties of chemicals necessary to know the danger, for example, phase transition, onset temperature in the decomposition reaction, etc., the reaction heat by the closed cell type thermal analysis method The present invention relates to a technique for sealing a cell used for measurement with a certain degree of sealing. That is,
The present invention relates to a technique for uniformly sealing a sealed cell for measuring a heat of reaction such as a phase transfer heat and a decomposition heat of a target chemical substance (hereinafter, referred to as a sample).

[Conventional technology]

There are two types of thermal analyzers used for measuring the thermal characteristics of chemical substances, for example, the thermal decomposition onset temperature, heat of reaction, and the like, based on their principles, a differential thermal analyzer and a differential scanning calorimeter. These were placed under the same temperature conditions as a sample cell containing a sample in a microcontainer (hereinafter referred to as a cell) and a control cell containing a control substance (usually using α-aluminum oxide). The analyzer records the temperature difference from the control cell, and the differential scanning calorimeter adjusts a built-in electric heater so as to eliminate the temperature difference from the control cell, and records the electric energy.

However, if there is any dissipation (leakage) of the cell contents during the measurement, it is recorded in the form of heat of vaporization, so that the correct calorific value of the decomposition reaction cannot be measured.

For this reason, what was devised is a structure that prevents leakage of cell contents by closing a cell body called a sealed cell.

As the material of the sealed cell, a metal having characteristics such as relatively high thermal conductivity, no reactivity with the sample, high strength, and low cost, such as aluminum, stainless steel, and silver, is used. .

In order to create this sealed cell, a sealed cell closure machine (hereinafter, referred to as a “container”) that converts rotational force into downward pressure
Rotary crimper) has been used.

FIG. 5 is a structural view of a conventional rotary crimper, and FIG. 6 is an enlarged view of a cuffed portion of the crimper of FIG. In these figures, the rotary crimper includes a crimper body 1 formed substantially in a U shape, a lever 2, a shaft mounting portion 3 provided on the crimper body 1, and a lid press-fitting mounted on the shaft mounting portion 3. And a sealing cell stand 7 on which the cell 6 is placed.

In such a rotary crimper, a cell 6 with a lid that has been weighed in advance is placed on a sealed cell table 7, a lid press-fitting shaft 4 is mounted on the shaft mounting section 3, and the lever 2 is rotated to cover the lid press-fitting. Push down the shaft 4 and push the lid into the cell 6. Next, the same operation is performed by replacing the lid press-fitting shaft 4 with the mouth-tightening shaft 5, and the sealing of the sealed cell is completed.

[Problems to be solved by the invention]

When using a conventional rotary crimper, lever 2
In order to apply a force in the rotation direction by operation, the tightening force by the individual who seals the cell varies, and a sealed cell sealed by a strong person and a sealed cell sealed by a weak person,
Even in a sealed cell closed by the same person, the degree of sealing was not constant due to the degree of force. For this reason, the mouth tightening is insufficient,
In some cases, the calorie measurement in the sealed container, which is the original purpose of the sealed cell, could not be performed due to leakage of the cell contents.

It is indispensable to create a sealed cell that is constant and has high airtightness by eliminating the difference in mouth closure due to individual differences that are likely to occur when using such a rotary crimper, in order to perform thermal analysis. That is.

The present inventors have intensively studied the problems with such a closed system having a closed cell, and by using a press-type crimper that easily applies force instead of a rotary crimper,
It has been found that even a person with a weak force can seal the sealed cell, and at the same time, by using a pressure gauge (or a load cell), obtains a sealed cell with good pressure resistance and a stable degree of sealing at a constant pressure.

SUMMARY OF THE INVENTION An object of the present invention is to provide a crimper for closing a closed cell mouth, which has a high sealing property and can obtain a certain degree of sealing regardless of individual differences.

[Means for solving the problem]

In order to achieve the above object, the present invention provides a press-type press that seals one cell body containing a sample and a lid with pressure when producing a sealed cell for thermal analysis, and a press-fit press attached to the press-type press. And a pressure gauge which is provided via a pressure sensor unit arranged in series with the axis of the sealed cell table on which the cell body is installed, and which displays a pressure at the time of sealing. Is a crimper for closing a closed cell.

[Action]

By mounting a pressure gauge at the bottom of the sealed cell when the sealed cell is closed, the sealed cell can be closed with a constant pressure at the time of closing and the reproducibility is extremely improved. In addition, since the crimper is a pressing crimper, even a weak person can easily seal the sealed cell with the necessary force easily. Therefore, the airtightness is high, and a certain degree of airtightness can be obtained irrespective of individual differences. [Examples] Hereinafter, the present invention will be specifically described with reference to one example of the drawings.

FIG. 1 is a configuration diagram of a press-type crimper with a pressure gauge according to an embodiment of the present invention, and FIG. 2 is an enlarged view of a mouth-closing portion of the press-type crimper of FIG. In these figures, the press-type crimper includes a crimper body 11 formed in a substantially U-shape and a lever.
12, a link mechanism 13 connected to the lever 12, a shaft mounting portion 14 provided on the crimper body 11 and connected to the link mechanism 13, and a lid press-fitting shaft 15 mounted on the shaft mounting portion 14.
Or a mounting part 18 to which a mouth-tightening shaft 16 and a pressure gauge 17 are mounted
And a sealed cell table 20 on which the cell 19 is placed. The pressure gauge 17 includes a pressure sensor 17a and a display unit 17b. The pressure sensor unit 17a is mounted on the mounting unit 18, and the display unit 17b is disposed on the operation side. This pressure sensor section 17a
Are arranged in series below the axis of the sealed cell table 20, and the cell 19 is placed on the sealed cell table 20. That is, the lever
By moving up and down 12, the shaft mounting portion 14 is moved up and down via the link mechanism 13, and the cover press-fitting shaft 15 or the
A press machine that presses or depressurizes the cell 19 with the pressure gauge 16 is provided.
It is displayed in b.

FIG. 3 is a view showing an example of the lid press-fitting shaft 15. In the figure, the lid press-fitting shaft 15 has a thin tip 15a for press-fitting the lid.
And a mounting portion 15b. The tip portion 15a preferably has a diameter of 1 to 3 mm and a length of 5 to 15 mm. Mounting part 1
5b is attached to the shaft attaching portion 14.

FIGS. 4 (a) to 4 (e) are cross-sectional views showing an example of the closing shaft 16. FIG. This mouth-tightening shaft 16 has a mouth-fastening portion 16a
And a mounting portion 16b. The closing part 16a is
Type inner as shown in the diagram (a) is hollowed out cone at an angle X _1, type inner as shown in FIG. 4 (b) is hollowed out frustoconical angle X _1, inside as shown in FIG. (C) Is a type with a cone cut out at angles X ₁ and X ₂ , and the inside is an angle as shown in FIG.
A mold with an elliptical surface processed at X ₁ and at an angle Y from the focal point,
As shown in FIG. 9E, there are types such as an elliptical surface at an angle Y from the focal point, and any type can be used in the present invention. In the drawings, where the play L is 0 to 5 mm, the angle X ₁ open cone, X ₂ is 10 to 170 °, the angle Y from the focal point of the ellipsoid is desirable that the 10 to 180 °.

According to the press-type crimper having such a configuration, at the time of closing the mouth, the cell 19 with the lid which has been weighed in advance on the sealed cell table 20 is used.
First, the cover press-fitting shaft 15 is attached to the shaft mounting portion 14, and the operator slowly pushes down the lever 12. The link mechanism 13 is linked to the pressing operation of the lever 12, and the lid press-fitting shaft 15 attached to the shaft mounting portion 14 pushes the lid into the cell 19 by the link mechanism 13. Next, the same operation is performed by replacing the lid press-fitting shaft 15 with the mouth-tightening shaft 16, and the sealing of the sealed cell is completed. At this time, the pressure at the time of producing the sealed cell is transmitted to the pressure sensor section 17a through the sealed cell table 20, and the pressure value is displayed on the pressure gauge 17. Therefore, the operator only has to read the value of the pressure gauge 17 and control the lever 12 operating force.

That is, according to the present invention, reproducibility is extremely improved by mounting the pressure gauge 17 on the bottom of the sealed cell when the sealed cell is closed, and by closing the closed cell with a constant pressure when closing the closed cell. In addition, since the pressing crimper is used, even a weak person can easily seal the sealed cell with a predetermined force (about 400 kgf) or more easily. This constant tightening force not only keeps the measurement conditions constant but also on a secondary basis, but the original design of the sealed cell clasp and the sealed cell, which often occurs in rotary crimpers. It is expected to maintain accuracy and performance over time.

Next, specific examples and comparative examples will be described. For the measurement, use a differential thermal analyzer, seal 10-25 mg of pure water under the following conditions, and measure the extrapolated endothermic onset temperature at which leakage starts under the condition of a temperature rise rate of 10 ° C / min. The cell withstand pressure was estimated from the relationship between water temperature and vapor pressure. Here, the relationship between temperature (T) and vapor pressure (P) is described in Chemical Handbook Revised 3rd Edition Basic Edition II (Maruzen)
The Harlacher-Braun equation for the vapor pressure of water described in was used.

In this Harlacher-Braun equation, ln (P) = 55.336−6869.5 / T−5.115ln (T) + 1.05P / T ² . Here, P: mmHg (height of mercury), T: K (absolute temperature), and ln represent natural logarithm.

[Example 1] Pure water was taken in a stainless steel sample cell having a diameter of 5 mmΦ and a height of 6 mm, the mouth was closed with a force of 450 kgf using a pressing crimper with a load meter, and differential thermal analysis was performed twice. . As a result, the extrapolated endothermic onset temperatures were 320 and 334 ° C.

[Example 2] Pure water was taken in a stainless steel sample cell having a diameter of 6 mmΦ and a height of 6 mm, the mouth was closed using a pressing crimper equipped with a pressure gauge with a force of 400 kgf, and differential thermal analysis was performed twice. . As a result, the extrapolated endothermic onset temperatures were 318 and 303 ° C.

Comparative Example 1 In a conventional rotary crimper shown in FIGS. 5 and 6, pure water was taken in a stainless steel sample cell having a diameter of 6 mm and a height of 5 mm. went. As a result, the extrapolated endothermic onset temperatures were 250, 320, 285
° C.

 Table 1 shows the results of comparison between the two.

That is, the press-type crimper of the present invention has higher hermeticity and a certain degree of hermeticity than the conventional rotary crimper.

In the present invention, the pressure gauge 17 only needs to be capable of detecting at least the pressure at the time of producing the closed cell and displaying the value, and may be capable of mechanically or electrically detecting and displaying the value.

Further, the pressing crimper is not limited to the link mechanism of the embodiment as long as it has a structure capable of applying a pressing force to the cell by operating the lever.

〔The invention's effect〕

As described above, according to the present invention, it is apparent that the use of a press-type crimper with a pressure gauge has higher sealing performance and a certain degree of sealing compared to the case of using a conventional rotary crimper. Can be obtained.

[Brief description of the drawings]

FIG. 1 is a configuration diagram of a press-type crimper with a pressure gauge according to an embodiment of the present invention, FIG. 2 is an enlarged view of a mouth-closing portion of the press-type crimper of FIG. 1, and FIG. 4 (a) to 4 (e) are cross-sectional views illustrating an example of a mouth-tightening shaft according to an embodiment of the present invention, FIG. 5 is a configuration diagram of a conventional rotary crimper, FIG. FIG. 6 is an enlarged view of a cuffed portion of the crimper shown in FIG. In the figure, 11 is the crimper body, 12 is the lever, 13 is the link mechanism, 14 is the shaft mounting part, 15 is the lid press-fitting shaft, 15a is the tip, 15b is the mounting part, 16 is the mouth-tightening shaft, and 16a is the tip Reference numeral 16b denotes a mounting portion, 16b denotes a mounting portion, 17 denotes a pressure gauge, 17a denotes a pressure sensor portion, 17b denotes a display portion, 18 denotes a mounting portion, 19 denotes a cell, and 20 denotes a sealed cell stand.

Claims (1)

(57) [Claims] 1. A press-type press machine for sealing a cell body containing a sample and a lid by manual operation of a lever via a link mechanism when preparing a sealed cell for thermal analysis. A pressure gauge mounted on a press machine, provided through a pressure sensor unit arranged in series with a shaft of a sealed cell base on which the cell body is installed, and displaying a pressure at the time of sealing. A manually operated crimper for closing the cell mouth.