JPH0623701B2 - Calorimeter - Google Patents

Description

Description: TECHNICAL FIELD The present invention relates to an improvement of a calorimeter for measuring the calorific value of solid and liquid substances, and in particular, in a calorimeter capable of directly recording the rise of the inner cylinder water temperature as the calorific value. , The measurement accuracy is improved and the structure is simplified.

Generally, a calorimeter for measuring the calorific value of solid and liquid substances, a fixed amount of a sample is enclosed in a bomb together with compressed oxygen for complete combustion, and this bomb is immersed in an inner cylinder containing a specified amount of water, In this outer cylinder, the sample in the bomb is burned by passing an electric current through the ignition wire of the bomb in the outer tub containing water at the same temperature as the inner cylinder water temperature, and the combustion heat is absorbed by the inner cylinder water, The calorific value is measured from the rise. In this case, the outer tub water heating device is provided in the outer tub, and the outer tub water temperature is increased in accordance with the temperature rise of the inner tub water, so that the temperature difference between the inner tub water and the outer tub water is substantially zero. In this way, the heat insulating effect is provided, the influence of the ambient temperature at the time of measuring the calorific value is removed, and the measurement accuracy is improved. The calorific value of such a calorimeter is expressed by the following equation.

Calorific value (cal) = {inner cylinder water amount (g) + equipment water equivalent (g)} x inner cylinder water rise temperature By the way, in such a calorimeter, the calorific value is proportional to the temperature rise of the inner cylinder water. Since it is measured by the relationship, if a temperature fluctuation factor from other than the inner cylinder is added, it naturally changes the apparatus water equivalent value, and the change amount of the apparatus water equivalent appears as a measurement error of the immediate heat value.

The apparatus water equivalent as used herein is defined to include all heat absorption factors including water in the inner tube of the apparatus system.

According to Japanese Patent Publication No. 59-34966, as a method for weighing a specified amount of water in an inner cylinder, a method of injecting water in an outer tank into the inner cylinder by means of a solenoid valve and its accompanying introduction pipe and liquid level relay However, in this case, the water in the outer tank to be injected into the inner cylinder is once guided to the solenoid valve in the air layer outside the outer tank, and again passes through the inlet pipe in the outer tank to the inner cylinder. It is structured to enter. However, in this method, the solenoid valve connected from the outer tank to the inner cylinder and a part of the introduction pipe are in a temperature environment other than the heat insulating structure, so that the temperature rise of the inner cylinder water should be measured correctly as a method of measuring the temperature rise. Even if the temperature difference of the outer tank water is manipulated to be substantially zero, even if the heat insulation effect is provided, the water equivalent of the device actually changes due to the influence of the part such as the solenoid valve which is not affected by the effect. It will be. Especially when it is desired to improve the measurement accuracy, the effect is not negligible. Normally, when measuring with this calorimeter, it is difficult to finely adjust the room temperature, and a fixed setting of ± 1 to 3 ° C is usually set. Therefore, in calorimetric measurement where the temperature rise is usually measured. It causes an error.

In the present invention, such a drawback of the conventional calorimeter is overcome, and a solenoid valve and an introduction pipe for introducing water from the outer tank to the inner cylinder are always provided with respect to the inner cylinder water temperature.
The accuracy of measurement is remarkably improved by installing it in the outer basin water that is adjusted within 5 minutes of 0 ° C and eliminating the influence from the surrounding environment other than the heat insulation structure to suppress the fluctuation of the water equivalent of the equipment. It is an object of the present invention to obtain a calorimeter which is improved and has an extremely simplified structure and is easy to operate.

That is, according to the present invention, in the calorimeter capable of directly recording the rise in the water temperature in the inner cylinder as the calorific value, the calorific value in which the electromagnetic valve for automatically weighing water in the inner cylinder is installed in the outer tank water. A total is provided.

Next, the present invention will be described with reference to the drawings.

In FIG. 1, reference numeral 1 is an outer tank, into which outer tank water 7 is charged. The outer tank has a stirrer 6 and a detector 8 for detecting the temperature of the outer tank water 7. In the outer tank 1, there is an intermediate tank 3 having an air layer 9, and in the intermediate tank 3, an inner cylinder 2 is provided. The inner cylinder 2 has a bomb 4 and a stirrer 5 for burning the sample, and the inner cylinder 2 is filled with water at the time of measurement. Therefore, the inner cylinder 2 is provided with an electrical contact 10 as a part of an inner cylinder water weighing device for weighing water, to which a liquid level relay 16 is connected, and further on the output side thereof. A solenoid valve 15 for injecting water into the inner cylinder 2 is fixed to the intermediate tank 3 and is connected to the inner cylinder 2 by an introduction pipe 19. In addition, the inner cylinder 2 has a detector 11 for detecting a temperature rise in the inner cylinder water and a temperature detector 11 'for adjusting the temperature of the outer tub water 7 to the same temperature as the inner cylinder water temperature.
Is provided. Reference numeral 12 is a lid of the intermediate tank 3.

The detector 11 for the water temperature in the inner cylinder is connected to the recorder 18 via the calorimeter 17. Further, the detector 11 'provided on the inner cylinder 2 is connected to the outer tank water temperature adjusting device 20 together with the detector 8 provided on the outer tank 1, and is connected to the solenoid valve 13 as its output side. Reference numeral 14 denotes a hot water tank, which is filled with heated water.

The calorimeter of the present invention has the above-described configuration. To operate the calorimeter, the bomb 4 is installed in the inner cylinder 2 and then the outer tank water 7 is put into the outer tank 1. Next, water having a predetermined temperature is produced by the outer tub water temperature adjusting device 20, and if the temperature of the injected water is lower than the preset temperature at this time, the solenoid valve 13 is automatically opened and the heated water is heated in the tub. It is injected from 14 and a predetermined water temperature is created.

Next, the outer tank water 7 adjusted to a predetermined temperature is introduced into the inner cylinder 2 by the inner cylinder water weighing device and weighed. First, the solenoid valve 15 is opened and the outer tank water is placed in the inner cylinder 2. When 7 is injected and the water surface reaches the electrical contact 10, a signal is sent to the liquid level relay 16 and the solenoid valve 15 is closed. Then, when a prescribed amount of water is weighed in the inner cylinder 2, the sample in the bomb 4 is burned to absorb the heat in the inner cylinder water. At that time, the inner cylinder water temperature rises with the release of heat, but in order to prevent the heat from escaping to the outside, the temperature of the inner cylinder water is read by the detector 11 'and the outer tub water temperature adjusting device 20 is used to The temperature difference with the detector 8 provided in the tank 1 is detected, and the solenoid valve 13 is opened so that the temperature difference between the inner cylinder water and the outer tank water is substantially zero, and the heated water is injected from the hot water tank 14. . The measurement of the water temperature in the inner cylinder ends when the combustion of the sample ends and the release of heat from the bomb 4 stops, but the temperature rise at that time is sent to the calorimeter 17 by the detector 11 and converted into a calorific value to be recorded. Recorded by 18. Although the measurement operation ends here, the water in the inner cylinder 2 is discharged into the outer tub 1 by opening the solenoid valve 15 in preparation for the next measurement.

In the present invention, the inner-cylinder water weighing device is a device composed of the electrical contact 10 and the liquid level relay 16 and the solenoid valve 15 connected thereto. FIG. 2 shows the details of the solenoid valve 15 which is a part of the apparatus.

2 is the side wall of the inner cylinder, and 3 is the side wall of the intermediate tank. 15
Is a solenoid valve, which is in series with a waterproof cover 21 and an introduction pipe 19; the introduction pipe 19 is connected to an outer tank and an inner cylinder via a solenoid valve 15.

Next, the structure and function of the device according to the present invention will be described in detail.

As mentioned above, this inner cylinder water weighing device also operates during a series of measurement operations, but only this part will be explained again in order of operation, first, when the temperature of the outer tank water is adjusted. Then, the solenoid valve 15 is opened and the water in the outer tank 1 is injected into the inner cylinder 2 by utilizing the head. When the water surface reaches the electric contact 10 provided in the inner cylinder 2, the liquid level relay 16
To the electromagnetic valve 15 to close the inner cylinder water weighing operation. When the inner cylinder water is discharged after the measurement is completed, the electromagnetic valve 15 is opened, and at the same time, the water in the outer tub 1 is also discharged into the outer tub 1.

With this structure, unlike conventional calorimeters, separate solenoid valves are not used for water supply and drainage of the inner cylinder, and
Since the solenoid valve 15 is directly fixed only to the intermediate tank 3 and the introduction pipe and the like are not fixed to the outer tank and can be moved together with the intermediate tank 3 in the outer tank, the structure and operation can be simplified.

On the other hand, in terms of the effect of improving the measurement accuracy, since the calorimeter is calculated from the formula of the above-mentioned principle, the solenoid valve connected to the inner cylinder is the air of the non-insulated environment outside the outer tank as in the conventional calorimeter. If it is installed in a layer, the water equivalent of the equipment will change and the calculated calorific value will include an error. But,
In the calorimeter according to the present invention, since the solenoid valve is installed in the well-controlled heat insulation structure in the outer tank water, the correct value is recorded without changing the water equivalent of the apparatus.

[Brief description of drawings]

FIG. 1 is a block diagram of an apparatus system of the present invention, and FIG. 2 is a perspective view of a row of apparatuses in a water introducing portion of an inner cylinder. 1 …… Outer tank 2 …… Inner cylinder 3 …… Intermediate tank 4 …… Bomb 5,6 …… Stirrer 8,11,11 ′ …… Sensor 13,15 …… Solenoid valve 14 …… Hot water tank 16 …… Liquid level relay 17 ... Calorimeter 18 ... Recorder 20 ... Outer tank water temperature controller

Claims (1)

[Claims] 1. An intermediate tank having an air layer is provided inside the outer tank, an inner cylinder is provided inside the intermediate tank, and a pump for burning a sample is provided inside the inner cylinder. With the specified amount of water contained in the inner cylinder, the sample is adiabatically burned in the pump, and the temperature of the outer tank water is adjusted so that the temperature difference between the inner cylinder water temperature and the outer tank water becomes zero. In a pump-type calorimeter capable of directly recording the amount of heat generated by adiabatic combustion of a sample as an increase in the water temperature in the inner cylinder while controlling it, the introduction pipe that supplies the outer tank water to the inner cylinder does not have to be through the outer tank wall A calorimeter characterized in that the electromagnetic valve for controlling the supply of outer tank water to the inner cylinder is directly fixed to the outer wall of the intermediate tank as a waterproof structure while being disposed through the intermediate tank wall and the inner cylinder wall.