JPH0643126A - Plumbing method for inner/outer tank in calorimeter - Google Patents

Abstract

PURPOSE:To shorten the measuring time for continuous heat generation without making a calorimeter larger in size by taking into account the plumbing method for the calorimeter. CONSTITUTION:In prior to the following heat generation measurement after the preceding measurement has been completed, the water in an inner tank is completely removed practically and then a specified amount of water whose temperature is lower than the set temperature is fed into an outer tank 14. Further, after the temperature in the outer tank became approximately same as the set temperature, a part of water in the outer tank is fed into the inner tank 12, thereby shortening the time necessary for removing/ feeding water in the inner and outer tanks and adjusting the set temperatures therein and reducing total measuring time.

Description

Detailed Description of the Invention

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a water supply / drainage method for an inner / outer tank in a calorimeter, and more particularly to an inner tank for accommodating inner tank water and a calorimeter bomb set to a predetermined temperature and an outer tank set to a predetermined temperature. An outer tank for containing water and a temperature adjusting means for adjusting the temperature of the outer tank water by following the temperature rise of the inner tank water are provided, and the heat of combustion of the sample in the calorimeter bomb is set within the set temperature. The present invention relates to a water supply / drainage method for an inner / outer tank in a calorimeter that absorbs water in the tank water and measures the calorific value of the sample based on the temperature rise value of the inner tank water.

[0002]

2. Description of the Related Art Calorimeters of the type described above are well known.
An example thereof is shown in Japanese Patent Laid-Open No. 4-15549. In this type of calorimeter, after measuring the calorific value of the sample, the inner and outer tank water are naturally higher than the set temperature. It is common practice to discharge water and then supply water to the inner and outer tanks to adjust the temperature to a preset temperature.

[0003]

By the way, in this type of calorimeter, it is advantageous that the calorimeter is as small as possible in consideration of transportation to the measuring place, installation area at the measuring place, handling of the calorimeter, and the like. And it is being requested by the general public. Also, in this type of calorimeter, the calorific value of the sample is repeatedly measured.Therefore, after the calorific value measurement is completed, the preparation period for the next measurement should be shortened as much as possible to shorten the calorific value measurement time. Has been requested.

However, in the calorimeter, as described above, all the inner and outer tank water whose temperature has risen after the measurement of the calorific value of the sample is once discharged, and then water is newly supplied to the inner and outer tanks. Since a means for adjusting the set temperature is adopted, it takes a considerable amount of time when the time for discharging and supplying the inner and outer tank water and adjusting the newly supplied inner and outer tank water to the set temperature are combined. I cannot answer the request for shortening the measurement time.

In order to meet such a demand, a means for increasing the diameter of the supply pipe, the discharge pipe, the supply / discharge valve, etc. of the inner / outer tank water to shorten the discharge time and supply time of the inner / outer tank water is conceivable. Due to these water supply / drainage means, there is a problem that the calorimeter becomes large and the measurement accuracy decreases. It is also possible to supply a large amount of constant temperature water that has been adjusted to a preset temperature to the inner and outer tanks to shorten the time required to adjust the temperature of the inner and outer tank water to the set temperature. Due to this, the calorimeter becomes larger due to this,
There is a new problem that goes against the demand for miniaturization of calorimeters.

Therefore, an object of the present invention is to improve the supply and discharge means of inner and outer tank water after the calorific value of a sample is measured and prior to the next measurement, so that the calorific value can be measured without increasing the calorimeter. To shorten the measurement time.

[0007]

DISCLOSURE OF THE INVENTION The present invention is an inner tank for accommodating an inner tank water set to a predetermined temperature and a calorimeter bomb;
An outer tub containing outer tub water set to a predetermined temperature, and a temperature adjusting means for adjusting the temperature of the outer tub water by following the temperature rise of the inner tub water, of the sample in the calorimeter bomb A method of water supply and drainage for the inner and outer tanks in a calorimeter that measures the heat generation amount of the sample based on the temperature rise value of the inner tank water by absorbing combustion heat, and the heat generation amount that is continuously performed after the heat value measurement is completed. Prior to measurement, after discharging substantially all of the inner tank water, a predetermined amount of water having a predetermined temperature lower than the set temperature is supplied to the outer tank so that the outer tank water has substantially the same temperature as the set temperature. In addition, a part of the outer tank water is supplied to the inner tank.

Further, the present invention is a method of supplying and draining water to and from the inner and outer tanks of the above calorimeter, wherein substantially all of the water in the inner tank is discharged before the measurement of the calorific value after the end of the calorific value measurement is completed. After draining a part of the bath water, a predetermined amount of water having a predetermined temperature lower than the set temperature is supplied to the outer bath to bring the outer bath water to a temperature substantially equal to the set temperature, and Part is supplied to the inner tank.

[0009]

In the water supply / drainage method of the present invention described above, the water temperature lower than the set temperature is substantially set by supplying water lower than the set temperature to the outer tank in a state where all or a large amount of the water in the outer tank higher than the set temperature remains. The temperature of the outer tank water is adjusted, and then a part of the outer tank water is supplied to the inner tank to form the inner tank water. For this reason, compared to a means of once discharging all the inner and outer tank water and then newly supplying all the inner and outer tank water, the discharge and supply time of the inner and outer tank water is significantly shortened, and the setting of the inner and outer tank water is set. The time required for adjusting the temperature is significantly shortened, and the time required for measuring the calorific value can be significantly shortened.

Further, in the water supply / drainage method of the present invention, the measurement time of the calorific value is significantly shortened. Therefore, in order to meet the request for shortening the measurement time, the supply pipe, the discharge pipe, the water supply / discharge pipe of the inner / outer tank water are provided. There is no need to adopt a means to shorten the discharge time and supply time of the inner and outer tank water by increasing the diameter of the valve etc., and supply a large amount of constant temperature water adjusted to a preset temperature to the inner and outer tanks Since it is not necessary to employ a means for shortening the time for adjusting the set temperature of the bath water, it is possible to prevent the calorimeter from increasing in size, and it is possible to meet the demand for miniaturizing the calorimeter.

In the calorimeter to which the water supply / drainage method of the present invention is applied, the total amount L of the inner / outer tank water, the discharge amount (supply amount) ΔL, the temperature difference Δt between the rising temperature of the inner / outer tank water after the measurement and the set temperature.
1. The relationship between the temperature difference Δt2 between the temperature of the water to be supplied and the set temperature is given by the following equations (1) and (2).

[0012]

(1) (L-ΔL) × Δt1 = ΔL × Δt2

[0013]

## EQU00002 ## .DELTA.t2 = (1 / .DELTA.L) .times. (L-.DELTA.L) .times..DELTA.t1 Therefore, in the above equations, L and .DELTA.L are constant, and .DELTA.t1 is the same kind of combustion sample and has a large calorific value. Since there is no difference, it is substantially constant. Therefore, it suffices to prepare the feed water having a temperature difference Δt2 lower than the set temperature. In addition,
When measuring the calorific value of the combustion samples of greatly different calorific values, it is possible to adopt a means for changing the drainage amount in response to the change of Δt1 each time. Further, when the supply water having a temperature difference Δt2 lower than the set temperature is a considerably low temperature, it is possible to increase the temperature of the supply water by increasing ΔL by a predetermined amount.

[0014]

DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS An embodiment of the present invention will be described below with reference to the drawings. FIG. 1 schematically shows a calorimeter adopting the supply / discharge method of the present invention. The calorimeter is the calorimeter body 10
And a water supply / drainage means 20 and a temperature control means 30. The calorimeter main body 10 includes a calorimeter bomb 11, an inner tank 12 that houses the bomb 11, an intermediate tank 13 that houses the inner tank 12, and an outer tank 14 that houses the intermediate tank 13. At the time of measuring the calorific value in the calorimeter main body 10, water (inner tank water) set to room temperature is housed in the inner tank 12 housing the bomb 11, and an air layer is formed between the inner tank 12 and the intermediate tank 13. And water between the intermediate tank 13 and the outer tank 14 is set to room temperature (outer tank water)
Are housed and sealed.

The supply / discharge means 20 is provided with a hot water tank 21, a cold water tank 22 and a drainage tank 23, and each of these tanks 21-2.
3 and a large number of pipes connecting the calorimeter main body 10, a large number of valves 24a, 24b ... And a large number of pumps 25a, 25b. In the supply / discharge means 20, while supplying water to the inner tub 12 and the outer tub 14 of the calorimeter main body 10 as will be described later, water in each of the inner and outer tubs 12 and 14 (inner tub water, outer tub water). Is discharged.

The temperature control means 30 is a first temperature setting means 31 for setting the temperature of the inner tank water, and a second temperature setting means for setting the temperature of the outer tank water.
A temperature setting means 32 and a temperature adjusting means 33 for adjusting the temperature of the outer tank water are provided. The first temperature setting means 31 is a known device that is connected to a temperature sensor 31a installed in the inner tank 12, measures the temperature of the inner tank water at the start of measurement and during measurement, and outputs the detection signal as the amount of heat generation. It is output to the measuring means, and the calorific value is measured by this. The second temperature setting means 32 is a temperature sensor 32a installed in the outer tub 14.
It is a well-known device that is connected to, and measures the temperature of the outer tub water at the start of measurement, outputs the detection signal to a predetermined electromagnetic valve, and controls the valve to set the outer tub water to a preset temperature, room temperature. Adjust to.

The temperature adjusting means 33 includes temperature sensors 31a,
A known device connected to 32a measures the temperature of the inner and outer tank water during measurement and outputs the detection signal to a predetermined electromagnetic valve, and controls the valve to control the temperature of the outer tank water. Is to follow the temperature rise of the inner tank water.

The measurement of the calorific value of the sample by the calorimeter constructed as described above will be explained. When the calorimeter is used for the first time or when the calorific value measurement is once suspended and then restarted, the valve 24a is first set. It is opened to supply a predetermined amount of water to the hot water tank 21 and heated by a heater (not shown) to obtain hot water having a constant temperature higher than room temperature. Next, the valve 24b is opened and a predetermined amount of water is supplied to the cold water tank 22 and cooled by a cooler (not shown) to obtain cold water having a constant temperature lower than room temperature. In addition, when the hot water and the cold water gradually decrease due to use, they are replenished each time and a constant amount of hot water and cold water at a constant temperature is constantly supplied to each tank 21,
Store in 22. This completes the preparation for measurement.

Next, in preparation for measurement, preparation for measurement is performed according to the following steps (1) to (4). (1) A predetermined amount of sample is contained in the bomb 11, high-pressure oxygen is injected, and the bomb 11 is accommodated in the inner tank 12 that constitutes the calorimeter main body 10. The inner tank 12, the intermediate tank 13, and the outer tank. 1
Seal 4 (2) Open the valve 24c to supply water from the water supply source to the outer tank 14
Supply in. When the supplied water is lower than room temperature which is the set temperature, the opening / closing operation of the valves 24d and 24e is controlled by the action of the second temperature setting means 32 to replenish the hot water in the hot water tank 21, and further the opening / closing of the valve 24f. The operation and the drive of the pump 25a are controlled to adjust the outer tub water to a preset temperature of room temperature. (3) When the temperature of the outer tank water is adjusted to room temperature and becomes stable, the valve 24g is opened and the pump 25b is driven to supply a part of the outer tank water into the inner tank 12 to obtain the inner tank water. Is a constant amount. (4) During this time, the valve 24 is operated by the operation of the first temperature setting means 31, the second temperature setting means 32 and the temperature adjusting means 33.
The opening / closing operations of d, 24e and 24f and the driving of the pump 25a are controlled so that the inner tank water and the outer tank water are accurately adjusted to the same temperature.

After the preparation for measurement, the sample is burned in the bomb 11 constituting the calorimeter body 10 to absorb the heat of combustion into the inner tank water, and the temperature sensor 31a detects the temperature of the inner tank water, which is not shown. A detection signal is output to the calorific value measuring means to measure the calorific value. During this time, the temperature of the outer tub water is raised by the action of the temperature adjusting means 33 following the temperature rise of the inner tub water,
Improves the measurement accuracy of calorific value. This completes the first measurement.

Next, in preparation for the second measurement, first the valve 24h is opened and the pump 25c is driven to discharge substantially all the inner tank water in the inner tank 12, and the valve 24i is turned on. When opened, a part (a fixed amount) of the outer tank water in the outer tank 14 is discharged. The method for discharging the inner and outer tank water, which comprises the above procedure, constitutes a part of the water supply / drainage method of the present invention. Then, the inner tank 12, the intermediate tank 13, and the outer tank 14
The lid is opened, the bomb 11 is taken out, the inside of the bomb 11 is degassed, and the cap is removed from the body of the bomb 11.

Next, a predetermined amount of the sample is placed in the bomb 11 and high-pressure oxygen is injected, and the bomb 11 is placed in the calorimeter body 1.
It is accommodated in the inner tank 12 which constitutes 0, and the inner tank 12 and the intermediate tank 1
3 and the outer tank 14 are sealed, and then water is supplied into the outer tank 14 and the inner tank 12. In this case, the valve 24f is opened and the pump 25a is driven to supply the cold water in the cold water tank 22 into the outer tank 14, while the opening / closing control of both valves 24d and 24e is performed by the action of the second temperature setting means 32. Hot water from the hot tub 21 is supplied into the outer tub 14 as needed, and the outer tub water is adjusted to the set room temperature. After the outer tub water is adjusted to room temperature and stabilized, the valve 24g is opened and the pump 25b is driven to supply a predetermined amount of outer tub water into the inner tub 12, and the temperature adjusting means 33 acts so that the inner and outer tub water is The temperature of is accurately adjusted to the same temperature. This completes the preparation for the second measurement. The above-mentioned water supply means for the inner and outer tank water constitutes another part of the water supply / drainage method of the present invention.

As described above, the water supply / drainage method of the present invention is a water supply / drainage method for the inner and outer tanks in the preparation process for the second and subsequent measurements, and the outer tank water in the outer tank 14 is higher than room temperature which is the set temperature. By supplying cold water lower than room temperature to the outer tank water at approximately room temperature in a state of being left in a large amount, a part of the outer tank water is then supplied into the inner tank 12 to be used as the inner tank water. is there. For this reason, compared with a means of once discharging all the inner and outer tank water and then newly supplying all the inner and outer tank water, the amount of water discharged to and from the inner and outer tanks is small and the supply and discharge time is significantly shortened. In addition, the time for adjusting the temperature of the inner and outer tank water to room temperature is significantly shortened, and the time for measuring the calorific value can be greatly shortened.

Further, in the water supply / drainage method of the present invention, since the measurement time of the calorific value is significantly shortened, in order to meet the request for shortening the measurement time, the supply pipe, the discharge pipe, the supply / discharge pipe of the inner / outer tank water are supplied. There is no need to adopt a means to shorten the discharge time and supply time of the inner and outer tank water by increasing the diameter of the balf, etc., and also to supply constant temperature water adjusted to a preset temperature to the inner and outer tanks to supply water to the inner and outer tank water. Since it is not necessary to employ a means for shortening the adjustment time to the set temperature, it is possible to prevent the calorimeter from increasing in size, and it is possible to meet the request for miniaturization of the calorimeter.

In the calorimeter, the calorific value can be accurately measured by the following method. That is, the value of the indicator that displays the amount of heat generation according to the temperature rise based on the signal detected by the temperature sensor 31a is G. When the accuracy is not so required, the value of G may be used as the calorific value, but in reality, an error is included due to each factor (room temperature, heat capacity of the apparatus, water temperature, etc.). In order to eliminate this error, the value of G is corrected based on the following formula (corrected correct value H). Using a standard sample whose calorie is known in advance, a relational expression (H = a · G + b) between the accurate calorific value H and the measured value G of the sample is obtained. In this case, the G value at that time is obtained by changing the weight of the standard sample (the H value changes). This is repeated several times to obtain the above relational expression between the H value and the G value. If the H value is calculated by substituting the measured value G of the measurement sample into this relational expression, this H value becomes the correct value of the corrected amount of heat.

[Brief description of drawings]

FIG. 1 is a schematic configuration diagram of a calorimeter adopting the water supply / drainage method of the present invention.

[Explanation of symbols]

10 ... Calorimeter body, 11 ... Bomb, 12 ... Inner tank, 13 ...
Intermediate tank, 14 ... Outer tank, 20 ... Supply / discharge means, 21 ... Hot water tank, 2
2 ... Cold water tank, 24a, 24b -... Valve, 25a, 25
b ... Pump, 30 ... Temperature control means, 31, 32 ... Temperature setting means, 33 ... Temperature adjusting means.

 ─────────────────────────────────────────────────── ─── Continuation of the front page (72) Hiroshi Kimoto, 3-3-22 Nakanoshima, Kita-ku, Osaka City, Kansai Electric Power Co., Ltd. (72) Koji Seike, 2-167, Taishi, Midori-ku, Nagoya 1 (72) Inventor Nobuhiko Ishida 2-611, Asahide, Midori-ku, Nagoya 1 (72) Inventor Takanori Soda 347-8, Kosei-cho, Okazaki-shi, Aichi

Claims (2)

[Claims] 1. An inner tank for containing an inner tank water set to a predetermined temperature and a calorimeter bomb, an outer tank for containing an outer tank water set to a predetermined temperature, and the outer tank water being the inner tank water. Of the sample in the calorimeter bomb to absorb the heat of combustion of the sample in the calorimeter bomb to generate heat of the sample based on the temperature rise value of the internal tank water. A method for supplying and draining water to and from the inner and outer tanks in a calorimeter for measuring the amount of heat, prior to measurement of the calorific value after the end of the calorific value measurement, at least substantially all of the water in the inner tank is discharged, and then to the outer tank. A calorimeter characterized by supplying a predetermined amount of water having a predetermined temperature lower than a set temperature to bring the outer tank water to substantially the same temperature as the set temperature and supplying a part of the outer tank water to the inner tank. Water supply and drainage method for inner and outer tanks in Japan. 2. Prior to the subsequent measurement of the calorific value after the end of the calorific value measurement, substantially all of the inner tank water is discharged and part of the outer tank water is discharged, and then the setting is performed in the outer tank. 2. A predetermined amount of water having a temperature lower than the temperature is supplied to bring the outer tank water to substantially the same temperature as the set temperature, and a part of the outer tank water is supplied to the inner tank. Water supply and drainage method for the inner and outer tanks of the calorimeter described in.