JPS59153156A - Calorimeter - Google Patents

Abstract

PURPOSE:To enable the common use of a thermoelectric element, to simplify the constitution of a calorimeter and to prevent the generation of the error caused by the characteristic difference of two thermoelectric elements, by constituting a symmetric specimen part having a reference specimen container receiving hole, a specimen container receiving hole and a fine gap while mounting the thermoelectric element to said fine gap so as to detect the temp. difference between both wall surfaces of said fine gap. CONSTITUTION:A specimen and heat receiving member 1 consists of a symmetric specimen part 5 having reference specimen container receiving hole 2, a specimen container receiving hole 3 and a fine gap 4, the heat receiving part 7 opposed to a heat generating part 6 and a heat transfer part 8 having a narrow cross-sectional area for connecting said heat generating part 7 and the aforementioned specimen part 5 and a thermo-module 9 for detecting the temp. difference between both wall surfaces of the fine gap 4 is inserted into said fine gap 4. Even if these is unbalance in thermal resistance in the same places between the heat generating part and the heat receiving part, heat can be uniformly supplied to the reference specimen 18 and the specimen 19.

Description

DETAILED DESCRIPTION OF THE INVENTION The present invention relates to calorimetric needles, particularly differential scanning calorimeters. As shown in FIG. 1, this type of calorimeter has a reference sample container S and a sample container C arranged in a heat bath a, and a thermoelectric element such as a thermo module between the containers A and C and the heat bath 8. d
, , d, and the sample '+gt' is heated by a heating element e, which is already known.

Since the thermal resistance between the reference sample container S and sample container C and the vast heating element 8 is not necessarily the same, it is difficult for the reference sample container and sample container C to receive heat evenly. The thermoelectric element di used for the reed and the container S and C, respectively.
, , and d generally have different characteristics, so it is important to obtain output signals corresponding to them even at the same temperature. Therefore, the conventional method had the disadvantage that it required differential scanning calorimetry with a high phase change.

The present invention provides differential scanning heating without such inconvenience! The purpose is to provide a standard test container storage hole, a sample container storage hole, and a symmetrical sample part with a slit formed between them, and a heat receiving part facing the 5 heating elements. and,
It consists of four small-area thermoelectric sections that connect the heat receiving section and the sample section.

The sample section, the heat receiving section, and the heat conducting section are all made of a thermally conductive material, and the sample heat receiving member is provided in the gap with a thermoelectric element inserted therein to detect the temperature difference between the two wall surfaces. It is assumed that the component is housed within the insulating shield.

Embodiments of the present invention will be described below with reference to the drawings.

FIG. 2 is a schematic sectional view of one embodiment of the present invention, and FIG. 3 is a perspective view of the sample receiver 2 heating member.

In Figure 2, (υ is the sample heat receiving member, and the sample heat receiving member (υ is the reference sample container storage hole (28 sample container storage hole (3) and the A symmetrical sample part (5) having the entire slit (4), a heat receiving part (7) facing the heating element (6), and the receiving part, @# (
It consists of a heat conductive part (8) with a narrow cross section and area connecting the front N pipe sample part (7) and the front N pipe sample part (8), and is made of a thermally conductive material. For example, a thermo module is inserted as a thermoelectric element (9) for detecting the temperature difference between both wall surfaces.

The sample heat receiving member (υ is the heat insulating material Q1 via the heating element (6)
4 on top! It has 1 heating element and 0 units! It is housed within the F'r heat shield (2).

The reference sample container storage hole (2) and the sample container storage hole (3) of the sample part (5) are both formed in a cone shape with a wide opening, and the container Q1 is inserted into the hole (2a). When fitted, it adheres well to the hole wall and easily receives heat from the circumferential surface of the container.

In Figure 3, αυ is a thermocouple that detects the temperature of the heat insulating shield (2) and the sample part (5), respectively, and its valley output is input to the difference amplifier αQ, and its output is inserted into the circuit of heating element 4. In addition to fc control e4i device αη, thermal shield (6
) and 1M degree M of the sample part (5)? , Therefore, there is no exchange of heat between the two, and the influence a# from changes in the heat in the outside world is avoided.

Although the RTf heating element (6) is not shown, a constant power control circuit or a constant current control circuit (when the resistance of the heating element is constant)
This prevents the heat generating cover of the first heating element (b) from being affected by fluctuations in the power supply.

Next, to explain the operation of this embodiment, when one heating element generates heat, the heat flowing into the heat receiving part (9) with a large area in contact with it is first throttled by the heat conducting part (8) with a narrow cross section. After that, the flow is divided equally to both sides of the a gap (4) of the symmetrical sample Pr part (5), and the reference sample '4 vessel (13aJ and sample container) inserted into each storage hole <2) (3) is (to the reference sample within 13 days) and Sample #+α 碍 are equally heated.

In this way, the sample Ql undergoes an endothermic or exothermic change, and the temperature around the sample container storage hole (3) changes to the reference sample container storage hole (2).
When the surrounding temperature drops or rises, the temperature difference is detected by the thermo module (9).

According to this example, it was possible to accurately memorize a temperature difference of 1/10,000°C.

In this way, according to the present invention, the heat received from the heat receiving part with a large area is once divided by the heat conducting part with a narrow @ area, and then the reference sample container storage hole part of the symmetrical sample part and the sample container storage hole are divided. Since the flow is divided into parts, even if there is an imbalance in thermal resistance depending on the location between the heating element and the heat receiving part, the total heat can be evenly supplied to the reference sample and the sample. Since the entire heat generating element is disposed between the hole and the sample container storage hole, the thermoelectric cable can be shared, which simplifies the construction and eliminates noise errors caused by differences in the characteristics of the two thermoelectric elements.

Furthermore, when using a liquid sample as a sample, a certain amount of -1i' is required, but the sample absorbs heat from the wall surface of the storage hole and uses an element to increase the average temperature from the bottom to the top of the sample. Because it detects temperature differences, it has the advantage of being able to measure more accurately than conventional methods that detect temperature sounds from the bottom of the container.

[Brief explanation of the drawing]

FIG. 1 is a schematic sectional view of a conventional calorimeter, FIG. 2 is a schematic sectional view of an embodiment of the present invention, and FIG. 3 is a perspective view of a sample heat receiving member thereof. (1)...Sample heat receiving member (2)...Reference sample container storage hole (3)...Sample container storage hole (4)...Slit (5)...Sample part (7)・Heat receiving part (
8)...Heat conduction part (9 loaves...Thermoelectric element (2)
...Insulation Shield % Applicant Makabe Riko Co., Ltd. Procedural Supplement to the Commissioner of the Japan Patent Office 1. Indication of the case 1982 Patent Application No. 26940 2. Name of the invention changed to 3. Person making the amendment Relationship to the case Patent applicant: Shinku Riko Co., Ltd. 4, agent: 7035 Nico Shinkyo Hill, 2-16-1 Shinbashi, Minato-ku, Tokyo
, IE+J of the amendment order (spontaneous) Kusunoki 7 of the "Detailed Description of the Invention" of the specification (Monday, Showa) Contents of the amendment (1) "Heat receiving part (9)" on page 5 of the specification, line 3 Section (7)”.

Claims (1)

[Scope of Claims] (1) A symmetrical sample portion having a reference sample container storage hole, a sample container storage hole, and an M gap formed therebetween, and a heat receiving portion facing two heating elements; the heat receiving portion and the sample portion; The heat receiving part, the heat receiving part, and the heat conducting part are all made of a heat conductive material, and the narrow gap detects the temperature difference between the two walls. The sample heat receiving member is provided with a thermoelectric element inserted therein, and the sample heat receiving member is housed within a heat insulating shield. The calorimeter according to item 1, characterized in that the calorimeter is formed in the range of the special FF. 3. The calorific value needle according to claim 1, wherein the heat insulating shield has a heating element, and the heating element is controlled so that the temperature difference between the heat insulating shield and the sample part is small. .