JPS59135356A - Liquid specimen container for ac calorimeter - Google Patents

Abstract

PURPOSE:To simplify preparing work and measurement, by a method wherein two cylinders respectively closed by good heat conductive plates at one ends thereof are superposed so as to provide a predetermined gap therebetween to form a gap part for receiving a liquid specimen while the space between two cylinders is brought to an air-tight structure and a signal taking-out thermoelectric element and a temp. measuring thermocouple are attached to the surface of at least one good heat conductive plate. CONSTITUTION:After a liquid specimen 8 is injected into the gap part formed by good heat conductive plates 3, 4 from the upper parts of cylinders 1, 2, a seal material 9 is interposed to the upper part of a flange plate 6 which is, in turn, covered with a lid plate 10 and both plates are clamped by bolts to form an air-tight structure. A temp. measuring thermocouple 11 and a signal taking-out thermocouple 12 are attached to the plate surface of the good heat conductive plate 4 in a spot-welded or adhered state. A liquid specimen container having the above mentioned structure is arranged in a hot bath and the good heat conductive plate 4 is irradiated with intermittent light from below. The output of the signal taking-out thermocouple 12 is measured by amplifying the same by a lock-in amplifier while recording the same by a recorder. Because this output is inversely proportional to specific heat as is known, specific heat is calculated from said output.

Description

[Detailed description of the invention] The invention also relates to a liquid sample container for a flow calorimeter.

In addition, the method of measuring specific heat using flow calorimetry has been gradually put into practical use in recent years because it allows the measurement of the specific heat of a sample at each temperature at small temperature intervals.

In this method, one surface of a sample is heated in an alternating current manner by intermittent irradiation with a t-lamp beam, and temperature changes in the entire sample are detected by thermometers attached to all surfaces of the sample. The sample has a thickness that is short relative to the wavelength of the heat wave, and the sample is made so that its temperature does not increase over time due to the heat wave, and changes in response to the heat wave. It is placed in connection with a heat bath with a predetermined thermal resistance.

Conventionally, the samples measured using this method were only solid samples such as metals and ceramics, but because of the above-mentioned superior characteristics, it can also be used to measure the specific heat of liquid and jelly-like living organisms. There is a possibility that it will be used.

In view of the above circumstances, it is an object of the present invention to provide a liquid sample container for use in a flow calorimeter, in which two cylindrical bodies each having one end closed with a thermally conductive plate are connected with a predetermined gap between them. A spacer made of wire is interposed between the two thermally conductive plates to form a liquid sample storage gap, and the space between the two cylinders is made airtight, and the thermally conductive plates are polymerized. The main feature is that an element for symbol extraction and temperature measurement heat output is attached to one side of the device.

The drawing shows a cross-sectional view of a liquid sample container according to an embodiment of the present invention.

In the drawing, (1) and (2) are concentric cylinders made of a material with relatively low thermal conductivity, such as stainless steel, each with a thermally conductive material such as phosphor bronze at its lower end. A guide plate (31(4)) is fixed, and a closing plate (5) and a collar plate (6) are fixed to the upper ends of the guide plate (31(4)).

The thermally conductive plates f3] (4) are made to face each other with a thin wire, such as a gold wire (7), arranged as a spacer so that a certain gap is formed between them in order to accommodate a liquid sample.

After injecting the liquid sample (8) from the upper part of the cylinder (1) <2) into the gap formed by the thermally conductive plate (3) (41), the gap space is evacuated and completely filled with helium gas. To make this possible, a sealing material (9) such as indium wire is interposed on the upper part of the flange plate (6), and a lid plate αQ made of stainless steel, for example, is covered and bolted to form an airtight structure.

A thermocouple aυ for temperature measurement and a thermocouple for signal extraction (6) are attached directly to the heat conductive plate (4) by spot welding or gluing. As the thermocouple (6) (6), one having a sufficiently smaller heat capacity than that of the sample (8) is used.

The liquid sample container having the above structure is placed in a heat bath under the above conditions like a known calorimeter, and intermittent light is irradiated onto the thermal conductive plate (4) from below. The temperature change of the liquid sample (8) caused by this intermittent light is
) The output sound of the signal extraction thermocouple (6) attached to the surface of the thermal conductive plate (4), which has the same temperature as that of the thermocouple (4), is amplified by a lock-in amplifier that uses the signal corresponding to the intermittent light as a reference signal. This output is inversely proportional to the specific heat, so the specific heat can be calculated from this output. In addition, the average temperature of the liquid sample (8) can be determined by amplifying the output of the temperature measuring thermocouple (b) attached to the heat conducting plate (4) with a DC amplifier and then recording it with a recorder. .

In this way, according to the present invention, two cylindrical bodies each having one end closed with a heat conductive plate are polymerized through a titration gap,
A spacer made of wire is interposed between the two thermally conductive plates to form the entire liquid sample storage gap, and the space between the two cylinders is made airtight, and one surface of the thermally conductive plate is Since a thermoelectric element for signal extraction and temperature measurement is installed on the floor, when measuring the specific heat of a liquid sample with a flow calorimeter, it is possible to easily fill a small fixed amount of the liquid sample, and it is also easy to use for measuring the specific heat. Preparation work is simple, as it only requires pouring the liquid sample into a container, and unlike solid samples, there is no need to bring a thermoelectric element into contact with the sample each time it is measured. Since the sample container is not easily placed in the heat bath, it is easy to place the sample container in the heat bath.

[Brief explanation of drawings]

The drawing shows a cross-sectional view of one embodiment of the invention. (11(2)...cylindrical body, (3) [4)...
・Heat conduction plate, (5)...occlusion plate, (6)...flange plate,
(7)...Spacer, (8)...Liquid sample, (9)
...Sealing material, α1...Lid plate, (6) (6)
...Thermoelectric element for temperature measurement and signal extraction. Patent applicant: X Ku Riko Co., Ltd. (2 others)

Claims (1)

[Claims] Two cylindrical bodies each having one end closed with a thermally conductive plate are overlapped with a predetermined gap between them, and a spacer made of wire is interposed between the two thermally conductive plates to form the entire gap for storing the liquid sample. A liquid sample container for an AC calorimeter, characterized in that the space between the two cylindrical bodies is made airtight, and a thermoelectric element for signal extraction and temperature measurement is attached to one surface of the heat conducting plate.