JPH09178683A - Sample cell for thermal analysis - Google Patents

Abstract

PROBLEM TO BE SOLVED: To obtain a sample cell by which heat can be measured precisely by a method wherein, in a thermal analysis, the sample cell is provided with a lid composed of a material whose light transmittance is high and with a container composed of a material whose thermal conductivity is high. SOLUTION: A material for a lid 1 is not limited to quartz, and a transparent material which can transmit light at a required wavelength sufficiently according to the optical characteristic of a sample 3 can be selected. The lid 1 is placed in a lid receiver part 4, the upper-part sidewall of a container 2 is bent to the inside, and the lid 1 can be fixed to the container 2. Thereby, it is possible to prevent the composition of the sample 3 from being changed when the low- boiling-point component of the sample 3 is heated and evaluated during a measurement. As a material for the container 2, aluminum, platinum, copper, gold, silver or the like whose reactivity with the sample 3 is small and whose heat conductivity is good is suitable. A result of high accuracy is obtained with the sample 3, to be measured, whose volatility is high. Thereby, when the thermal characteristic in the light-heat complex reaction of the sample 3 with volatility is measured, it is possible to prevent the vaporization of the sample and a change in its composition, and a quantity of heat can be measured precisely.

Description

Detailed Description of the Invention

[0001]

TECHNICAL FIELD The present invention relates to the thermal analysis of a sample under the condition where a photochemical reaction or a photo-thermal combined reaction such as a photo-isomerization reaction or a photo-curing reaction of a UV-curable resin is in progress. Regarding the sample cell used.

[0002]

2. Description of the Related Art Recently, due to advances in optical fiber manufacturing technology, the use temperature of ultraviolet curable resin under ultraviolet irradiation has risen in the manufacturing process of optical fiber, and the ultraviolet curable resin under high temperature and ultraviolet irradiation is used. The elucidation of the thermal characteristics of is an important issue. On the other hand, the basics of thermal analysis for material science Yasutoshi Saito (March 1994 Kyoritsu Publishing Co., Ltd.) 60
Although various sample cells for thermal analysis are described on pages 65 to 65, there is no description of a sample cell suitable for thermal analysis of a reaction involving light and heat simultaneously, which meets the above-mentioned object.

[0003]

While using a sample cell for thermal analysis made of a material such as platinum having good thermal conductivity which has been conventionally used in differential thermal analysis and the like, a sample which is easily volatilized is irradiated with light. When the thermal characteristics were measured at a high temperature, the sample was volatilized during the measurement and the composition of the sample was changed, which made accurate thermal analysis difficult. On the other hand, a conventional cell made of a material that transmits ultraviolet rays, such as fused silica, has been used by paying attention to its excellent heat resistance. Irradiation is possible, but poor thermal conductivity made accurate measurement difficult.

[0004]

According to the present invention, in a sample cell in which a measurement sample for thermal analysis is put and used for measuring thermal characteristics, the portion of the container which is in contact with the thermal analysis device has a thermal conductivity such as aluminum or platinum. The problem was solved by using a high-quality material and using a material such as quartz that transmits light through the lid. Incidentally, although there is a description of a quartz container in the above-mentioned document, this is used as a supplement to high temperature measurement because an aluminum container cannot be used at 600 ° C. or higher. It is not intended for general use.

Specifically, according to the invention of claim 1, the lid portion made of a material having a high light transmittance for irradiating light while preventing volatilization of the sample and the material having a high heat conductivity are used. It is a sample cell for thermal analysis characterized in that it is composed of a container part. The invention according to claim 2 is characterized in that the material having a high light transmittance is quartz.
The sample cell for thermal analysis described in 1. In the invention according to claim 3, the material having high thermal conductivity is aluminum, platinum, gold,
The sample cell for thermal analysis according to claim 1, wherein the sample cell is silver or copper. The invention according to claim 4 is the sample cell for thermal analysis according to claim 1, wherein the lid and the container can be fixed so as to be airtight.

[0006]

In the present invention, the container portion in contact with the calorimeter is made of a metal having high thermal conductivity, and the lid portion is made of a material such as transparent quartz, so that the light of the volatile sample can be reduced. When measuring the thermal characteristics during the reaction involving heat and
Since the thermal characteristics can be measured while avoiding the volatilization of the sample and the change in the composition, accurate heat measurement becomes possible.

[0007]

BEST MODE FOR CARRYING OUT THE INVENTION Embodiments of the present invention will be described in detail below with reference to the accompanying drawings. In the description of the drawings, the same elements will be denoted by the same reference symbols, without redundant description.

FIGS. 1, 2 and 3 show a sample cell for thermal analysis according to the present invention. FIG. 4A shows the thermal characteristics of the epoxy resin obtained as a result of scanning differential thermal analysis using the sample cell for thermal analysis according to the present invention shown in FIG. Figure 4 (b) shows
As a comparative example, the result of thermal analysis using a conventionally used sample cell for thermal analysis is shown.

An embodiment of the present invention will be described with reference to FIG. The present example is a sample cell for thermal analysis for analyzing a sample having a particularly high volatility. In FIG. 1, reference numeral 1 denotes a lid, which has a diameter of 4.4 mm, a thickness of 0.2 mm, and is made of quartz glass capable of transmitting ultraviolet rays. The lid 1 is not limited to quartz, and a transparent material that sufficiently transmits light of a required wavelength can be selected according to the optical characteristics of the sample 3.
Reference numeral 2 denotes a container portion of the sample cell, which has a diameter of 4.2 mm and a depth of 1.0 mm, and the diameter of the upper portion is 4.5 mm larger than that of the lower portion so that the lid 1 can be stored.
Is composed. Place the lid 1 on the receiving portion 4 of the lid,
The lid 1 can be caulked and fixed to the container 2 by bending the upper side wall of the container 2 inward. As a result, it is possible to prevent the low boiling point component of the sample from evaporating due to heating during the measurement and changing the composition.

As a material for the container 2, generally, aluminum, platinum, copper, gold, silver, etc., which have low reactivity with the sample and good thermal conductivity, are suitable.

Numeral 3 is a measurement sample, and the more volatile the sample, the more accurate the result can be obtained as compared with the conventional cell.

FIG. 4 shows the thermal characteristics of the UV curable epoxy resin 3 measured using a differential scanning calorimeter using the cell shown in FIG. As the ultraviolet curable epoxy resin 3 to be measured, an uncured liquid resin having high viscosity was used. For the measurement, the UV-curable epoxy resin 3 was used 10 times.
Only the amount of mg was put in the sample cell, the temperature was changed from room temperature to 100 ° C., and the calorific value was measured by a differential thermal analyzer. The measurement result is shown in FIG. 4 (a) by plotting the heat generation amount on the vertical axis and the temperature on the horizontal axis. Also, as a comparative example, under the same conditions,
FIG. 4 shows the result of measurement of the thermal characteristics of the UV curable epoxy resin 3 using a conventional platinum sample cell without a lid.
(B).

As is apparent from FIG. 4A, when the sample cell according to the present invention is used, a clear peak due to the heat of reaction appears, but a conventional sample cell without a lid. In the case of using, a slight undulation is recognized on the high temperature side as shown in FIG. 4 (b). Therefore, it can be seen that the use of the sample cell of the present invention enables extremely accurate measurement of thermal characteristics.

In the above embodiment, a gap is provided between the lid 1 and the sample 3 to prevent heat from escaping, thereby improving the measurement accuracy.

In this case, the height of the side wall of the container 2 is adjusted or the amount of the sample 3 to be put in the container 2 is adjusted so as to be in close contact with the lid 1 so as to block the air and prevent volatilization. Is also possible.

If the volatility of sample 3 is not very high,
The upper side wall of the container 2 is not bent to fix the lid 1 to the inside, and the measurement sample 3 is put into the container 2 as shown in FIG.
It is also possible to carry out the measurement with the lid 1 placed on the receiving portion 4 of the lid of the container 2 only. Also in this case, the lid 1 prevents the sample 3 from volatilizing, and the portion of the container 2 having excellent thermal conductivity efficiently transfers the reaction heat to the thermal analyzer, which is more accurate than the conventional sample cell. You can get high results.

Another embodiment will be described with reference to FIG.
In the present embodiment, when the volatility of the measurement sample 3 is not so high and it is necessary to avoid contact with air, the lid 1 and the measurement sample 3 are brought into close contact with each other, and the quality of the sample is altered by oxidation without being exposed to air. This is a sample cell for thermal analysis, which is suitable for performing thermal analysis while preventing volatilization of components. The part of the container 2 is the same as that of the first embodiment, but the part of the lid 1 has an outer diameter of 3.8 m.
It is made of quartz glass with m and a thickness of 0.6 mm. It is also possible to use those in which the thickness of the lid is variously changed according to the volatility of the measurement sample 3. Also in this case, the lid 1 prevents volatilization of the sample, and the portion of the container 2 having excellent thermal conductivity efficiently transmits the reaction heat to the thermal analyzer, which is more accurate than the conventional sample cell. The result can be obtained.

[0018]

As described above, the portion of the sample container that comes into contact with the calorimeter is made of metal having a high thermal conductivity, while the lid is made of transparent material such as quartz. When measuring the thermal characteristics of the sample having the property during the photo-thermal combined reaction, the amount of heat can be measured while preventing volatilization of the sample and changes in the composition, so that accurate heat measurement is possible.

[0019]

[Brief description of the drawings]

FIG. 1 is a diagram showing an example of a sample cell for thermal analysis according to the present invention.

FIG. 2 is a view showing a case used in the sample cell for thermal analysis shown in FIG. 1 without fixing a lid and a container.

FIG. 3 is a diagram showing an embodiment of a sample cell for thermal analysis of a type according to the present invention in which a lid and a measurement sample are brought into close contact with each other for measurement.

4 is a diagram showing thermal characteristics obtained by performing a differential thermal analysis on the ultraviolet curable epoxy resin 3 using the cell shown in FIG. FIG. 4 (a) shows the result of measurement using a sample cell for thermal analysis according to the present invention, and FIG. 4 (b) shows the result of measurement using a conventional sample cell for thermal analysis as a comparative example. .

[Explanation of symbols]

 1: Lid of sample cell for thermal analysis 2: Container part of sample cell for thermal analysis 3: Measurement sample 4: Receiving part of lid

 ─────────────────────────────────────────────────── ─── Continuation of the front page (72) Inventor Masashi Sato 1 Taya-cho, Sakae-ku, Yokohama-shi, Kanagawa Sumitomo Electric Industries, Ltd. Yokohama Works

Claims (4)

[Claims] 1. A sample cell for thermal analysis, comprising a lid part made of a material having a high light transmittance and a container part made of a material having a high thermal conductivity in the thermal analysis. 2. The sample cell for thermal analysis according to claim 1, wherein the lid portion made of a material having a high light transmittance is made of quartz. 3. The heat according to claim 1, wherein the portion of the container made of a material having high thermal conductivity is made of a metal material such as aluminum, platinum, gold, silver, or copper. Sample cell for analysis 4. The thermal analysis according to claim 1, wherein a side wall of an upper portion of the container is bent inward to fix the lid to the container so that the lid and the container are airtight. Sample cell for