JPH01215305A - Automatic distillation testing devide for chemical product or the like - Google Patents

Abstract

PURPOSE:To save manpower by using a sensor to detect the initial boiling point, distillation temp., distillate amt., end point, etc., and using a small-sized electronic computer to prepare a distillation curve at the time of conducting a distillation test of a chemical product. CONSTITUTION:When the distillation test of a chemical product is conducted, a sensor is used to measure the initial boiling point, distillation temp., distillate amt., end point, etc., and a small-sized electronic computer is used to prepare a distillation curve. The signal of distillation temp. measured by a resistance bulb 1 is sent to a transducer 3 through an amplifier 2 to obtain a digital signal which is inputted to the small-sized electronic computer 4. The beam of light emitted from a light source 6 fixed to a receiver 5 is received by a light receiving part 7 to detect the distillate amt., etc. The signal is transduced into a digital signal in the amplifier unit 8 provided with an amplifier and a transducer, and inputted to the computer 4. A distillation curve is prepared in the computer 4 from both signals, and inputted to a printer 9. As a result, the manpower spent by an analyst can be saved, and a more accurate measured value can be obtained.

Description

DETAILED DESCRIPTION OF THE INVENTION (Field of Industrial Application) The present invention relates to an apparatus for automatically performing distillation tests on chemical products and the like.

(Prior art) Distillation test methods for chemical products, etc. are based on the Japanese Industrial Standards (JI
S) Specified in No. K-0066.

For this specification, for example, in the case of a gas heating type, a device as shown in Figure 2 is used, and according to the heating rate shown in the test conditions, the initial boiling point, the relationship between distillation amount and temperature (distillation curve), the end point,
The method for determining the amount of remaining liquid is described.

In addition, in FIG. 2, the liquid sample is placed in a flask 21 and evaporated by being heated with a gas burner 22.
It condenses in a condensation bath 23 and the receiver 25 is in a water bath 24.
taken in The distillation temperature in this distillation operation is measured by a thermometer 26.

(Problem to be solved by the invention) In the conventional method specified by JIS, it is necessary to measure the distillation temperature and distillation amount at the same time. There is a need to be present, and it is desired to save labor.

In other words, according to the JIS regulations, (1) the time from the heating time to the initial boiling point, (2) the time from the initial boiling point to the distillation amount of 5%, and (3) the amount of time remaining in the flask after 5% distillation. (4) The time required for the remaining volume in the flask to reach the end point from 5 ml is specified in detail depending on the sample, and normally this distillation operation takes 20 to 30 minutes. During this time, the two analyzers cannot leave the distillation tester. Furthermore, the results of distillation tests are usually plotted on a graph of the relationship between distillation temperature and distillation volume, but this also requires a lot of effort.

For this reason, distillation tests for chemical products and the like require a lot of time using multiple analytical tools, and labor saving has become an important issue.

(Means for Solving the Problem) As a result of studying how to save labor in distillation tests for chemical products, etc., which require a lot of labor as described above, the inventors have developed a method for measuring distillation temperature, distillation volume, etc. using sensors. However, the present inventors have discovered that if a distillation curve is created using a small computer, labor can be efficiently saved and the present invention has been achieved.

That is, the present invention is characterized in that when performing a distillation test on a chemical product, the initial boiling point, distillation temperature, distillation amount, end point, etc. are measured using a sensor, and a distillation curve is created using a small computer. This is an automatic distillation testing device for chemical products, etc.

In the present invention, a distillation tester specified in JIS K-0066 is used, and each data is measured by the following method to create a distillation curve.

FIG. 1 is a diagram showing the measurement principle of the present invention. In FIG. 1, a signal of distillation temperature measured by a resistance temperature detector 1 is sent to a converter 3 via an amplifier 2, converted into a digital signal, and input to a small computer 4 manually. Further, the light receiving unit 7 detects the amount of distillation etc. using the light beam from the light source unit 6 attached to the receiver 5, and the signal is converted into a digital signal in the amplifier unit 8 equipped with an amplifier and a converter and sent to the small computer 4. is input.

A distillation curve is created from both signals in the small computer 4 and output to the printer 9. Note that the distilled amount can also be measured using ultrasound as described later.

A resistance temperature detector is usually used to measure the distillation temperature. The resistance temperature detector 1 has a shape as shown in FIG. 3, for example, and has a platinum wire 32 built into a hard glass 31, and a lead wire from a terminal 33 is connected to an amplifier. Platinum wire is usually Q, 1m
A diameter of about m is used, and the operating temperature range is 0 to 350.
It is ℃. This measurement accuracy is significantly higher than that of a glass thermometer specified by JIS.

For example, the following two methods are used to detect the amount of distillate.

(1) Measurement is performed by utilizing the fact that when the distillate enters the optical path, the energy at the light receiving section decreases. For example, with a structure as shown in FIG. The amount of distillation is measured by an optical sensor located on the right side of the light receiving section 43.As shown in the figure on the right, inside the light source section and the light receiving section, the light source 45 and sensor 46 are moved in parallel by a scanner motor 47, and the light receiving section is The liquid level in the container is detected.This signal is sent to the amplifier unit by a lead wire 44.

(2) For example, the structure is as shown in FIG. 5, and an ultrasonic sensor oscillator 52 is provided on the upper part of the receiver 51, and the ultrasonic sensor detects the reflected waves of the intermittently emitted ultrasonic waves on the distillate surface and the time intervals. The amount of distillation is measured by measuring with an oscillator and converting it into a signal proportional to the distance from the liquid surface with the amplifier unit 53.

To measure the initial boiling temperature, as shown in FIG. 6, a light beam from a light source 63 is passed through the end of a condensing tube 62 located in the upper part of a receiver 61, and the light beam is detected by a sensor 64. Further, the end point temperature can be detected from the jump in the measured temperature.

A distillation curve is created from the distillation temperature and distillation amount stored in a small computer. Note that the distillation temperature is corrected for atmospheric pressure according to JIS.

(Effects of the Invention) By using the distillation test device of the present invention, distillation tests for chemical products, etc. can be automatically performed, resulting in significant labor savings in analytical tools and more accurate measurement results. It will be done.

As a result, the number of man-hours required for the analysis tool in the distillation test is reduced, the cost of analysis is reduced, and highly accurate measurement values can be obtained, so that the present invention has great industrial significance.

[Brief explanation of the drawing]

FIG. 1 is a diagram showing the measurement principle of the present invention, and FIG. 2 is an example of a conventional distillation test apparatus specified in JIS. FIG. 3 is a diagram showing the structure of the resistance temperature detector used in the present invention, and FIG.
The figure shows how to measure the distillate amount using an optical sensor.
FIG. 5 is a diagram showing a method of measuring the distillate amount using an ultrasonic sensor oscillator, and FIG. 6 is a diagram showing a method of detecting the initial distillation temperature. Patent applicant Mitsubishi Gas Chemical Co., Ltd. Agent Patent attorney Sadafumi Kobori Figure 1

Claims (3)

[Claims] (1) When conducting distillation tests on chemical products, the initial boiling point, distillation temperature, distillation volume, end point, etc. are measured using sensors, and a distillation curve is created using a small computer. Automatic distillation testing equipment for products, etc. (2) An automatic distillation testing device for chemical products, etc., as set forth in claim 1, which passes a light beam from a light source to a receiver and measures the amount of distillation using an optical sensor. (3) An ultrasonic sensor oscillator is installed in the upper part of the receiver, and the amount of distillation is measured from the waves reflected from the distillate surface of the ultrasonic waves emitted intermittently. automatic distillation test equipment