JPS59170795A - Defferential thermal or scanning calorie analysis device - Google Patents

Abstract

(57) [Summary] This bulletin contains application data before electronic filing, so abstract data is not recorded.

Description

DETAILED DESCRIPTION OF THE INVENTION (a) Industrial application field This invention is a method of heating a sample and a thermally stable reference material (T, ie, α-alumina powder) side by side at a constant rate under equivalent conditions. The present invention relates to a differential scanning calorimeter that performs constant or quantitative analysis by measuring the temperature difference or energy difference between a sample and a reference material due to heat absorption or heat generation in the sample.

(4) Prior art differential thermal analysis (DTA) involves arranging the sample to be measured and a thermally stable reference material and heating them at a constant rate in a furnace with good temperature distribution. By measuring (iCJ and sample temperature TCC) and recording it, the thermal properties of the sample can be determined. It detects and measures the temperature imbalance that occurs when the sample absorbs heat during the process and generates one heat per unit compared to the reference material. The heat flow type detector is designed to be strictly proportional to the temperature difference, and a small thin heater is installed below the thermocouple to detect changes in heat absorption or heat generation in the sample. Compensate the heat with a small heater, that is, (DTA
There is also a heat compensation type that uses a small heater to adjust the heat so that the temperature difference between the two is always balanced and zero (similar to that in which the sample and reference material are heated at the same time). By the way, the shape of the thin thermocouple plate of the differential scanning calorimeter used in the conventional differential thermometer is shown in a plan view and a front cross-sectional view, respectively, in Figures 5-1 to 8. Shown as Fifth
In the current dumbbell-shaped model shown in Fig. 6 and Fig. 6, the space between the thermocouple R plate and the furnace acts as a thermal barrier, making it difficult for heat to diffuse from the thin plate to the surroundings. Since the heat inflow path to the substance side is narrow and it is difficult for heat to be transferred between them, changes in the amount of heat caused by heat absorbed by the sample can be measured with high accuracy. Moreover, since the weight of the thin thermocouple plate is small, and therefore the heat capacity of the system is small, even more sensitive measurements can be performed. However, due to its special shape, it is difficult to maintain a constant heat flux, and it is mechanically fragile. -The disk-shaped ones shown in Figures 7 and 8 are structurally strong, but they do not have a thermal barrier in the sense mentioned above, and as can be seen from their shape. Changes in heat amount due to heat absorption and absorption of the sample are easily transmitted to the reference material side. Furthermore, the heat capacity of the thermocouple thin plate is large, and as a result, sensitivity may decrease and quantitative performance may be lost.

In addition to what is shown in Figure 9, there is also a type of thermocouple that is constructed by vapor deposition on a ceramic substrate, but this produces a small amount of temperature interference between the sample and the reference material. Heat is transferred to the substrate, leading to diffusion of changes in heat amount due to heat absorption and heat absorption by the sample, resulting in a decrease in sensitivity.

T,! Purpose This invention solves the problems described above in the prior art.
Capable of measuring changes in calorific value with high sensitivity, quantitatively, and stably.
Furthermore, the purpose of this invention was to provide a structurally strong differential thermal or differential scanning calorimetry analyzer.

B) Configuration The present invention has a configuration that combines the advantages of conventional devices. In other words, the differential thermometer and differential scanning calorimeter according to the present invention include: - A thin plate molded from thermocouple material and having a mounting part for the sample on one side and a reference material on the other side at symmetrical positions; and - On the sample side. Differential heating or differential scanning calorimetry, which is equipped with a thermocouple for measuring temperature and the temperature difference between the sample side and the reference material side, and a furnace surrounding the thermocouples and heating the sample and the reference material. The analyzer is characterized in that the thin plate is disk-shaped, circular slits are provided so as to surround each mounting portion on the thin plate surface, and heat inflow passages are formed at two or more locations in each of the slits. By making the thin disk shape in this way, a predetermined strength is ensured, and at the same time, circular slits are provided to surround the sample and reference material placement areas, respectively, and these serve as thermal barriers.

And the heat capacity of the system was reduced. The heat then flows through the narrow heat inflow passages formed in each slit, making it difficult for the heat to be transferred.

(e) Examples Next, embodiments of the invention will be described.

The 17th is a front sectional view of the 2nd differential thermal analyzer.
Figure 9 is a plan view of the thin plate part in the device according to the present invention, Figures 3 and 4 are respectively [3-3) and (4-
4') is a sectional view. Thin plate (111 is chromel plate,
Using thermocouple materials such as aluminum plate, platinum plate (the one shown is chromel plate).

For example, it is molded into a disk shape with a thickness of 01 to 0.15 mm. And the thin plate (at the symmetrical position of 111).

Placement section 04 for sample (121 and reference material (13))!
, +151 are provided, and their mounting portions 114i,
(A circular slit is arranged to surround 151.Circular slit) The width of +161 is 9, for example, O, l-
It should be about 1mm. The circular slits (161) may be single as shown in the figure, or may be double or more. Each circular slit f161 has two (1, 1 or more (the illustrated one has 4) heat 17jt entrance passages f171). The width dimensions of the circular slots lJ, y l- (thermal barrier space 06) and the heat inlet passages (171) can be trimmed during fabrication to adjust the sensitivity and baseline stability.

In addition, the thin plate fi11. Placement part (141, (151) on the surface
teeth! In order to facilitate the installation of the sample cell, etc., it may be formed into a concave or convex shape (see FIG. 8).

The thin plate (111) is held with its peripheral edge in contact with the inner wall of the furnace 181.
The heat uniformly transmitted through IIIF flows into the sample u2 and the reference material (131) through the heat inflow passage (]9 provided in the two circular slits (thermal barrier spaces).In addition, inside the furnace αB0) Atmospheric gas flowing through the space rises through one circular slit (16). In the figure, [19] is a thermocouple, (A) is alumel, and (C) is chromel.

(F) Effect This invention has the configuration as described above, the heat capacity of the ν thermocouple part is small, and the furnace and sample.

The higher the thermal resistance between the sample and the reference material, the higher the sensitivity. Since the thermal resistance at Q,=KIT can be regarded as constant within the measurement temperature range, quantitative properties are improved. By adjusting the width dimensions of the heat barrier space and the heat inflow passage, it is possible to stabilize the base 2-in.

Furthermore, it was possible to provide a device with sufficient mechanical strength from a structural standpoint.

[Brief explanation of the drawing]

FIG. 1 is a front cross-sectional view of a differential thermal analyzer, FIG. 2 is a plan view of a thermocouple thin plate portion in the device according to the present invention, and FIGS. 3 and 4 are c 3-3'> ,
(This is a 4-4'l sectional view.
The figures show a plan view and a front cross-sectional view of a conventional device, respectively. 11... Thin plate 12... Sample 1
3... Reference material 14.15... Placement part 16... Circular slit 17... Heat inflow passage 18... Furnace 19. −・・・Thermocouple agent Patent attorney Takeshi Mamiya, Electrician゛1] [1・−
Figure 2 Figure 1 Figure 5 Figure 6 Figure 2 Figure 3 Figure 41. '1 7 Figure 8 Procedural amendment +1/+ August 3, 1995 [1 Director General of the Office of the Chief Justice 1, Indication of the case 1, Phase 58 I1 Patent Application No. 45157 2,
Name of the invention Differential thermal or differential scanning calorimetry analyzer 3, Person making the amendment Relationship to the matter Patent applicant II +j1 378 Roots Funatocho, Kawaramachi-dori Nijo, Nakagyo-ku, Kyoto City Name) (199) Shimadzu Corporation 8, Contents of amendment - (1) The scope of claims is amended as shown in the attached sheet. (2) The phrase "circular slit" on page 5, line 11 of the specification is corrected to "slit." (3) In the 2nd and 3rd lines of page 7 of the specification, following the statement ``It may be molded in a concave or convex manner (see Fig. 8),'' the following phrase is inserted. "In addition, in this embodiment, the shape of the square is circular, but it does not change the gist of the present invention if it is made into a triangle, quadrilateral, polygon, etc." 9 Correction of catalog of documents with threads Claims...1 Circular 2, Claims (revised) A thin plate molded from thermocouple material and having a sample on one side and a reference material on the other side in symmetrical positions, and a thin plate on the sample side. In a differential thermal or differential scanning calorimetry analyzer, which is equipped with a thermocouple for measuring the temperature of the sample and the temperature difference between the sample side and the reference material side, and a furnace surrounding the thermocouples and heating the sample and the reference material gold. , wherein the thin plate is disk-shaped, slits are provided so as to surround the mounting portion on the surface of the thin plate, and heat inflow passages are formed in two or more of the slits, or Differential scanning calorimeter.

Claims (1)

[Claims] A thin plate made of thermocouple material with a sample on one side and a reference material on the other side at symmetrical positions, and for measuring the temperature on the sample side and the temperature difference between the sample side and the reference material side. In a differential thermal or differential scanning calorimetry analyzer comprising a thermocouple and a furnace surrounding the thermocouple and heating a sample and a reference material, the thin plate is disk-shaped and a mounting portion on the surface of the thin plate is provided. A differential thermal or differential scanning calorimetry analyzer characterized in that circular slits are provided so as to surround each slit, and two or more thermal secondary passages are formed in each of the slits.