JP3945608B2 - Sample container for thermal analysis and manufacturing method thereof - Google Patents

Description

[0001]
BACKGROUND OF THE INVENTION
The present invention relates to a sample container for storing a sample to be subjected to thermal analysis and a method for manufacturing the same.
[0002]
[Prior art]
Conventionally, thermal analyzers such as TG (Thermogravimetry), DTA (Differential Thermal Analysis), DSC (Differential Scanning Calorimetry) and the like are known. In these thermal analyzers, when a sample is a volatile substance or a substance that generates gas by thermal decomposition, it is used for thermal analysis in a state where the sample is sealed in a sample container so that measurement can be performed under high pressure. Is done.
[0003]
Conventionally, as the sample container, as disclosed in Japanese Utility Model Publication No. 61-6335, one having a structure in which a lid body is press-fitted into a container body that accommodates a sample and the container body is sealed is known. Further, as disclosed in JP-A-63-317752, there is known a structure in which the inner peripheral surface of the lid is in close contact with the outer peripheral surface of the opening of the container body.
[0004]
[Problems to be solved by the invention]
However, with respect to each of the conventional sample containers described above, if the inside of the container becomes a high pressure, for example, 5 MPa or more due to a change in the characteristics of the sample accommodated therein, the internal gas may leak out and accurate thermal analysis may not be possible. was there.
[0005]
The present invention has been made in view of the above-described problems, and an object of the present invention is to provide a sample container that can prevent internal gas from leaking outside even when the internal atmospheric pressure becomes high.
[0006]
[Means for Solving the Problems]
To achieve the above Symbol purpose of the sample container thermal analysis according to the present invention comprises a container body inside surface includes a sample storage chamber for the sample to generate gas due to a temperature change is accommodated in contact with said sample, said container in the sample container thermal analysis and a lid is mounted to the body covering the sample receiving chamber, it is attached to the container body of the lid by an intervening member made of softer noble than the lid and the container body The lid is attached to the container body by press-fitting with the surface covered .
[0007]
According to the sample container for thermal analysis, the softer interposition member is interposed in the press-fitting portion between the container main body and the lid, so that high-pressure gas in the sample storage chamber can be reliably prevented from leaking to the outside. This is because the intervening member can prevent the formation of a fine gap between the container body and the lid from the beginning, and even when the container body and the lid are deformed by the internal high pressure, This is considered to be because the formation of voids can be prevented by the presence of the interposed member.
[0008]
In thermal analysis sample container according to the present invention, the interposed member Ru precious metal der. Here, the noble metal is a noble metal having a normal meaning, and is any of gold, silver, platinum group (Ru, Rh, Pd, Os, Ir, Pt), or an alloy thereof.
[0009]
In the sample container for thermal analysis according to the present invention, the interposition member is preferably formed on the surface of the press-fitting portion of the lid. The film formation is to form a film, and specifically, can be achieved by coating, plating, ion plating, or any other film forming method. In addition, interposing the interposition member itself is not limited to the film forming method as described above. For example, a method of press-fitting each other with a noble metal foil simply placed between the container body and the lid is also possible. Conceivable.
[0010]
In the following, the manufacturing method of the sample container thermal analysis according to the present invention, a sample generating a gas by temperature changes housed in contact with the inner surface of the container body into the sample storage chamber in the container main body, further the sample In the manufacturing method of the sample container for thermal analysis comprising covering the storage chamber with a lid , the sample is put into the sample storage chamber, and then the cover body is made of an intermediate member made of a noble metal softer than the container main body and the lid. The sample storage chamber is sealed by press-fitting the lid into the container main body in a state where the surface to be mounted on the container main body is covered .
[0011]
According to this method for producing a sample container for thermal analysis, since a softer intervening member is interposed in the press-fitting portion between the container body and the lid, the high-pressure gas in the sample storage chamber is transferred to the outside in the completed sample container. It is possible to reliably prevent leakage. This is because the intervening member can prevent the formation of a fine gap between the container body and the lid from the beginning, and even when the container body and the lid are deformed by the internal high pressure, This is considered to be because the formation of voids can be prevented by the presence of the interposed member.
[0012]
DETAILED DESCRIPTION OF THE INVENTION
FIG. 1 shows an embodiment of a sample container for thermal analysis according to the present invention. The sample container 1 shown here has a container body 2 provided with a sample storage chamber R in which a sample S is stored, and a lid 3 attached to the opening 4 of the container body 2 connected to the sample storage chamber R. The lid 3 is inserted into the opening 4 of the container body 2 while being press-fitted into the opening 4 of the container body 2, that is, pressed by an appropriate pressure. An interposition member 6 is formed in a film shape, that is, a film is formed on the surface of the press-fitted portion, that is, the outer peripheral portion of the lid 3.
[0013]
The sample S is, for example, a Class 5 dangerous substance according to the provisions of the Fire Service Law, that is, a substance that generates gas by evaporation or thermal decomposition, such as a self-reactive substance, and this is heated in a sealed container. The atmospheric pressure in the sealed container becomes a high pressure of 5 MPa or more, and in some cases, 8 MPa or more.
[0014]
The container body 2 is formed into a bottomed cylindrical shape with, for example, stainless steel. The lid 3 is formed of, for example, stainless steel in a disk shape with a small bottom surface (lower surface in FIG. 1) and a large ceiling surface (upper surface in FIG. 1). Further, the interposition member 6 is formed into a film having a uniform thickness by an arbitrary film forming method such as coating, plating, ion plating, etc., using gold as a precious metal, for example.
[0015]
When preparing the sample container 1 for thermal analysis, first, the sample S is put into the sample storage chamber R as indicated by the arrow A, and then the lid 3 is placed in the sample storage chamber R as indicated by the arrow B. Press fit into the opening. Thereby, as shown in FIG. 2, the sample container 1 for thermal analysis of the structure where the sample S was accommodated in the sample storage chamber R sealed by the lid 3 is completed. In a normal operation, the lid 3 is pressed using an appropriate pressing jig so as to be pressed straight onto the container body 2.
[0016]
In some cases, the sample S to be subjected to the thermal analysis generates a gas due to a thermal change, and therefore, the inside of the sample storage chamber R may be at a high pressure, for example, about 8 MPa or more. In the sample container 1 of the present embodiment, the lid 3 formed of stainless steel, which is a hard metal, and the container main body 2 formed of stainless steel are not directly brought into contact with each other, but gold that is a soft material between them is used. Is interposed between the lid 3 and the container main body 2 in a highly accurate sealed state, so that gas leakage from the inside of the sample storage chamber R is prevented. The interior can be maintained at a very high pressure with almost complete prevention.
[0017]
Further, even if the container body 2 and the lid 3 are deformed by the internal pressure, no gap is formed between the container body 2 and the lid 3 due to the action of the interposition member 6, and the sample is also observed from this surface. Gas leakage from the storage chamber R can be prevented, and the inside of the sample storage chamber R can be held at a very high pressure.
[0018]
FIG. 3 shows a main part of a heat flux type DSC apparatus which is an example of a thermal analysis apparatus which is an example of use of a sample container according to the present invention. The DSC apparatus shown here has, for example, a cylindrical heating furnace 8 for heating the measurement sample 7a and the reference sample 7b, and a programmed temperature control for controlling the temperature rise or cooling of the measurement sample 7a and the reference sample 7b according to a certain program. It has a circuit 9, a DC amplifier 11, a cold junction temperature compensator temperature linearizer 12, a heat quantity correction circuit 13, a recording unit 14 using a pen recorder, and the like. Each of the measurement sample 7a and the reference sample 7b is accommodated in the sample container 1 according to the present invention.
[0019]
The heating furnace 8 is formed of a metal material such as silver, and a heater 16 for heating is embedded inside the peripheral wall. The heater 16 is controlled by the programmed temperature control circuit 9 to generate heat. On the inner surface of the peripheral wall of the heating furnace 8, a heat sensitive plate 17 made of platinum or the like for supplying heat from the heater 16 to the measurement sample 7a and the reference sample 7b is provided, for example, by brazing. The sample containers 1 containing the sample 7a and the reference sample 7b are arranged at intervals.
[0020]
The programmable temperature control circuit 9 controls the temperature of the heating furnace 8 by controlling the heat generation of the heater 16 on the basis of the output signal of the control thermocouple 18 in which the temperature measuring point is placed in the heating furnace 8, that is, temperature information. . Further, temperature measuring points of temperature measuring thermocouples 19 and 21 are respectively attached to the portions of the heat sensitive plate 17 corresponding to the measurement sample 7a and the reference sample 7b, and the output ends of these thermocouples are connected to the DC amplifier 11 and the cooling point. It is connected to the contact temperature compensator temperature linearizer 12.
[0021]
When a thermal analysis measurement is performed on the measurement sample 7a, if a thermal change such as transition or melting occurs in the measurement sample 7a, a temperature difference occurs between the measurement sample 7a and the reference sample 7b, and the temperature A thermoelectromotive force is generated corresponding to the difference. Then, the thermoelectromotive force is sent to the DC amplifier 11 where it is amplified, and the amplified signal is sent to the heat quantity correction circuit 13. In the heat amount correction circuit 13, the heat amount necessary for the heat amount balance to be generated is obtained based on the temperature difference, and the heat amount information is sent to the recording unit 14.
[0022]
On the other hand, a thermoelectromotive force corresponding to the temperature of the measurement sample 7a is sent to the cold junction temperature compensator temperature linearizer 12, and the thermoelectromotive force is sent to the recording unit 14 in a state of being compensated based on the cold junction temperature. . In the recording unit 14, the heat quantity information sent from the heat quantity correction circuit 13 and the temperature information sent from the cold junction temperature compensator temperature linearizer 12 are recorded on paper or other recording material with a temporal relationship, Thereby, the thermal analysis result regarding the measurement sample 7a is obtained.
[0023]
The measurement sample 7a is stored in the sample container 1 as shown in FIG. 2, that is, the sample container 1 having a structure in which the lid 3 is press-fitted into the container main body 2 via the interposition member 6 made of gold or the like. Even when the inside of the sample storage chamber R becomes a high pressure, for example, about 8 MPa or higher due to a thermal change of the sample 7a, the interposition member 6 provides a highly accurate sealed state between the lid 3 and the container body 2. Thus, gas leakage from the inside of the sample storage chamber R can be prevented almost completely, and the inside thereof can be maintained at a high pressure.
[0024]
Further, even if the container body 2 and the lid 3 are deformed by the internal pressure, no gap is formed between the container body 2 and the lid 3 by the action of the interposition member 6, and the sample is also observed from this surface. Gas leakage from the storage chamber R can be prevented, and thus the inside of the sample storage chamber R can be held at a high pressure.
[0025]
(Other embodiments)
The present invention has been described with reference to the preferred embodiments. However, the present invention is not limited to the embodiments, and various modifications can be made within the scope of the invention described in the claims.
[0026]
For example, in the embodiment shown in FIGS. 1 and 2, the interposition member 6 is formed in a film shape with gold on the outer peripheral surface of the lid body 3, that is, the surface of the press-fitting portion, that is, the interposition member 6 is formed in other forms. It can also be formed of a noble metal material such as silver or platinum.
[0027]
In addition, the interposition member 6 is not necessarily formed in a film shape on the surface of the press-fitting portion of the lid 3 by a film forming method. For example, when the lid 3 is press-fitted into the container body 2, a gold foil is formed between them. It is also possible to employ a method in which both members are press-fitted in a state where the interposed member 6 is sandwiched, that is, in a state where the interposed member 6 is interposed.
[0028]
In addition, the interposition member 6 is not necessarily provided on the lid 3, and can be provided on the surface of the press-fitting part of the container body 2, that is, in the vicinity of the opening 4.
[0029]
FIG. 3 illustrates the case where the sample container for thermal analysis according to the present invention is applied to a DSC apparatus. However, the sample container for thermal analysis according to the present invention is applied to other thermal analysis apparatuses such as a DTA apparatus and a TG apparatus. Of course, it is also applicable.
[0030]
In addition, the container body and the lid are not necessarily formed of stainless steel, but can be formed of copper or any other metal. Moreover, depending on the case, a container main body and a cover body can also be formed with materials other than a metal. Further, the container body and the lid are not necessarily formed from the same material, and they can be formed from different materials.
[0031]
【The invention's effect】
According to the sample container for thermal analysis and the method for producing the same according to the present invention, since a softer interposition member is interposed in the press-fitting portion between the container main body and the lid, a high-pressure gas of 8 MPa or more in the sample storage chamber Can be reliably prevented from leaking outside. Thereby, it became possible to perform thermal analysis measurement under a high pressure condition of 5 MPa or more without any trouble.
[Brief description of the drawings]
FIG. 1 is a sectional view showing an embodiment of a sample container for thermal analysis according to the present invention in an exploded state.
2 is a cross-sectional view showing a state in which the sample container for thermal analysis in FIG. 1 is assembled.
FIG. 3 is a cross-sectional view and a circuit block diagram illustrating an example of a DSC apparatus which is an example of a thermal analysis apparatus.
[Explanation of symbols]
DESCRIPTION OF SYMBOLS 1 Sample container 2 Container main body 3 Cover body 4 Opening 6 Interposition member 7a Measurement sample 7b Reference sample 8 Heating furnace 16 Heater 17 Thermal plate 18, 19, 21 Thermocouple R Sample storage chamber S Sample

Claims (3)

A sample for thermal analysis, which has a sample storage chamber in which a sample that generates gas due to a temperature change is stored, has an inner surface in contact with the sample, and a lid that is attached to the container main body and covers the sample storage chamber In the container,
The lid body is attached to the container body by press fitting in a state where the surface of the lid body to be attached to the container body is covered with an intermediate member made of a noble metal softer than the lid body and the container body. Sample container for thermal analysis. Oite to claim 1, wherein the interposed member thermal analysis sample container, characterized in that it is formed on the surface of the press-fitting portion of the lid. A method for producing a sample container for thermal analysis in which a sample that generates gas due to a temperature change is stored in a sample storage chamber inside a container body so as to be in contact with the inner surface of the container body , and the sample storage chamber is covered with a lid. In
The sample is put into the sample storage chamber, and then the lid is covered with the container in a state where the surface of the lid attached to the container body is covered by an interposition member made of a noble metal softer than the container body and the lid. A method for producing a sample container for thermal analysis, wherein the sample storage chamber is sealed by press-fitting into a main body.

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