JP2637771B2 - Automatic coloring tester for chemicals - Google Patents

Description

DETAILED DESCRIPTION OF THE INVENTION [Industrial Application Field] The present invention relates to a chemical automatic coloring test apparatus for inspecting the properties of chemical products by coloring.

[Conventional technology]

In the case of certain products in the chemical industry, if the final product is further manufactured using this as a raw material, the presence or absence of impurities that affect the delicate properties of the final product such as color, texture, odor, etc. is measured. Things need to be done.

However, impurities which cause this are often complicated and subtle, which cannot be detected by ordinary measuring means (for example, gas chromatography).

If this is measured by a coloring test, the properties may be easily and quickly confirmed in some cases.

As such a test method, for example, there is a method such as JIS-K2421 "Test method for aromatic hydrocarbons", and as test target samples, polyhydric alcohols, phenols, ketones and the like are widely used.

In these test methods, the usual measurement method is to put a sample in a glass instrument having a specified shape, maintain the sample at a predetermined temperature, add a predetermined color test, perform a constant mixing, and obtain a mixture of the obtained mixed solution. Compare the degree of coloring visually with the standard coloring solution,
Or, it is common to measure the transmittance of the light with a photometer, and this entire operation has been conventionally performed by a human.

[Problems of the prior art]

However, the coloring test of chemical products is reproducible unless the type of reagent, container shape, mixing ratio of sample and reagent, test start temperature, mixing method and strength, liquid temperature at mixing, etc. are correctly observed. It is very difficult to get data.

For example, in ASTM-D848 “Sulfuric acid coloring test of industrial aromatic hydrocarbons”, the sample was added to 7 ml of sulfuric acid to add 2 ml.
8 ml, stopper and hold the whole container by hand for 5 to 40 seconds.
Shake vigorously to make 150 round trips over a distance of 10 inches.・ ・
Operations such as "" must be performed strictly, and skill is required.

In addition, since the substance to be handled often generates a large amount of heat during mixing depending on the type of test, it is difficult to shorten the time of this test method, and improvement in productivity has been strongly desired.

The present invention has been completed in order to solve such problems, and has as its technical object to eliminate the need for skill in testing and to improve productivity.

[Means for solving the problem]

In order to solve such a problem and always perform an accurate test, there is no other way than to make the fine mixing conditions conventionally performed manually by an automatic device, but it is performed by hand with ordinary glassware. Automating the entire measurement operation as it is is labor-intensive and ineffective, and the whole apparatus is only complicated.

The inventors of the present invention have made various studies, and as a result, have completed an automatic apparatus by accumulating various changes and improvements as described below.

That is, in the present invention, as shown in FIG. 1, an automatic sample measuring device 1 for measuring a liquid sample such as phenol, glycol, or aromatic hydrocarbon, and an automatic reagent for measuring sulfuric acid as a coloring reagent A measuring instrument 2, a pure water supplying section 6 for supplying pure water, an injection pipe 44 connected to the automatic sample measuring instrument 1, an injection pipe 45 connected to the automatic reagent measuring instrument 2, and the pure water supplying section A mixing tank 3 having an injection pipe 43 and a discharge pipe 46 connected to the mixing tank 6 for mixing the liquid sample and the coloring reagent; and coloring the liquid in the mixing tank 3 by using the mixing tank 3 as a cell 75. A colorimeter 4 for measuring the degree and an operation control unit 5 are provided. The operation control unit 5 introduces pure water from the pure water supply unit 6 into the mixing tank 3 and then performs colorimetry with the pure water. 4 is calibrated, and after the calibration, the pure water is discharged from the discharge pipe 46. Is introduced into the mixing tank 3, a coloring reagent is introduced from the automatic reagent measuring device 2 into the mixing tank 3, and the coloring degree is measured by the colorimeter 4 after the coloring reaction is completed. An automatic coloring test device was used.

The above is the configuration of the present invention, and the specific configuration will be described below.

(A) First, as the automatic sample measuring device 1, an automatic valve is provided at each of both ends on an inlet side and an outlet side of a tube, and a measuring tube for measuring a predetermined amount by using a volume in the tube between the automatic valves is exemplified. Yes, or use a pump or other negative pressure source to pump or inject a liquid sample into the weighing vessel, or connect a liquid sampling tube to the line through which the chemicals flow, and An example in which an automatic valve is provided on the way and a predetermined amount of liquid sample is introduced into the measuring container by opening and closing the automatic valve can also be exemplified. In the case of using a measuring container, a storage tank for storing a liquid sample is installed above the measuring container, a discharging nozzle toward the measuring container is provided below the storing tank, and an automatic valve is provided for the discharging nozzle. The liquid sample in the storage tank may be allowed to fall naturally into the measuring container by opening and closing the automatic valve. Here, it is a requirement that the liquid sample can be automatically introduced into the measuring container, and such a case is not limited to the above example.

The measuring method by the automatic sample measuring device 1 can be controlled by time when the amount of liquid sample flowing into the measuring container per unit time is known. For example, there is a method in which the opening time of the automatic valve is set to a fixed time when the flow rate in the pipe from the line is known. As another measuring method, there is a method in which a sensor for detecting a liquid surface is provided in a measuring container, and the liquid surface of a liquid sample stored in the measuring container is detected at a predetermined height and measured. Examples of the sensor to be used include a switch that floats a float in a liquid sample and turns on when the float rises, and a photoelectric switch that detects a liquid level by a combination of a light emitting unit and a light receiving unit.

When the measurement in the measuring container is completed, it is necessary to transfer the liquid sample in the measuring container to the mixing tank 3. Examples of the method include a method of transferring, a method of pumping and transferring by a pump or the like using a suction pipe, a method of providing a cock that can be automatically opened and closed at the lower part of the measuring container, and a method of opening the cock and transferring by natural fall. In the case of the measuring tube, the liquid sample that has been measured can be transferred to the mixing tank 3 by opening the automatic valve on the outlet side.

(B) Next, the coloring reagent is sulfuric acid, and the automatic reagent measuring device 2 for supplying the coloring reagent to the mixing tank 3 includes the above-mentioned automatic valves at both ends on the inlet side and the outlet side of the tube. And a metering tube for measuring a predetermined amount with the internal volume of each automatic valve tube can be exemplified as a preferred embodiment. If a predetermined amount of the coloring reagent can be introduced into the mixing tank 3, the above-mentioned (a) Other measuring instruments as exemplified in the above section can also be applied.

(C) The liquid sample from the automatic sample meter 1 and the coloring reagent (sulfuric acid) from the automatic reagent meter 2 are mixed in the mixing tank 3. The mixing procedure is as follows: the liquid sample is put first, and the coloring reagent is put later, and vice versa.
There are two cases.

In addition, mixing usually requires a stirring operation. In the conventional manual analysis, a cylindrical container such as a cylinder or a test tube is used as the mixing tank 3 to mix and stir a liquid sample and a coloring reagent. Is caused by reciprocating vibration of the container, inversion, etc., but this mixing / stirring mode is not suitable for an automatic apparatus. Therefore, in the present invention, rotary stirring is preferably used. As an example of the rotational stirring, a method of providing a rotor made of a magnetic material that does not cause a chemical reaction with a liquid sample or a coloring reagent in the mixing tank 3 and rotating the rotor with a rotating magnetic field outside the mixing tank 3 is used. Can be exemplified. Further, an air motor type rotary stirrer as described in the following embodiments can be exemplified. Further, as a simple rotary stirring, a method in which a stirring rod is inserted into the mixing tank 3 and the stirring rod is rotated by a driving device such as a motor can be exemplified.

It is preferable that the mixing tank 3 has a structure capable of maintaining a target temperature so as to be compatible with a test method in which the temperature at the start of mixing or during mixing is specified. For example, a heater with an automatic temperature controller is attached to the mixing tank 3, or the mixing tank 3 is placed in an outer container, and the space between the outer container and the mixing tank 3 is inertized at a predetermined temperature. Means for circulating a fluid can be exemplified.

The strength of the mixing conditions that are different for each test method is adjusted by changing the stirring speed, the addition speed of the reagent, and the temperature of the mixing tank 3.

(D) Next, in the conventional method, there is also a test method using visual judgment as a means for measuring the degree of coloring, but in the present invention, this was replaced with the colorimeter 4 and automated.

As the colorimeter 4 suitable for automation, a photoelectric type and a flow cell type are preferable. In this case, the selection of the photometric wavelength is very important.

The mixing tank 3 and the colorimeter (cell 75) of the colorimeter 4 are integrated and used for both purposes, and the mixing tank 3 has a function as a colorimeter (cell 75) of the colorimeter 4. ing. In the colorimetric test using the colorimeter 4, the colored liquid sample in the mixing tank 3 is not moved from the mixing tank 3 without moving the mixing tank 3, that is, the cell 75.
It is performed in.

(E) When the colorimetric test is completed by the colorimeter 4, it is necessary to discharge the tested liquid sample. However, usually, the liquid sample is temporarily discarded and stored in a waste tank, and is collectively disposed at a later date.

The discharge from the cell 75 of the colorimeter 4, that is, from the mixing tank 3 to the waste tank may be performed by a natural fall from a pump or a nozzle with a valve as described above.

(F) Depending on the test method or the properties of the test substance (liquid sample), it is necessary to keep the measurement environment temperature constant. For example,
It is a substance that solidifies at room temperature.

If this is necessary, the entire apparatus may be housed in a temperature-controllable housing.

(G) The delivery of the liquid sample and the coloring reagent between the respective parts is performed by the above-described pump, suction by a negative pressure source, pressure feeding by a pressurized gas source, natural fall, etc. , Suction by a pressurized gas source, and natural fall. Switching of an automatic valve is necessary for delivery of a liquid sample or the like, and the automatic valve is controlled by the operation control unit 5 to open and close.

The liquid sample may be heated to a predetermined temperature as needed. In such a case, the entire apparatus may be placed in a heating atmosphere, or the liquid sample container, the mixing tank 3 and the like may be heated. Various heat sources can be used as the heating source, but using heating nitrogen from a chemical plant is preferable in terms of safety and economy.

The material used for the apparatus is a material that satisfies all of the solvent resistance, corrosion resistance, and heat resistance.

(H) Examples of the operation control unit 5 that controls the operation of each unit described above include a sequence control by a sequencer and a computer control method by a microcomputer.
If necessary, it is not possible to measure the liquid sample with a measuring tube,
Various sensors detect liquid leaks in each part, overflow of the cell part of the colorimeter 4, decrease in nitrogen flow rate for heating, abnormal temperature in the apparatus, decrease in pressure of the gas for pumping, etc. And the like.

[Action]

 The device of the present invention operates in the following order.

First, the colorimeter 4 is calibrated using pure water instead of a liquid sample (the light transmittance in the case of pure water is set to 100% transmittance). Next, the liquid sample is circulated through the circulation path of the apparatus by the same operation as the main measurement described below, and each part is washed.

Next, in this measurement, the automatic sample weighing device 1 is operated by a command from the control device, and the liquid sample is automatically weighed. The weighed liquid sample is sent to the mixing tank 3.

Before or after this, sulfuric acid as a coloring reagent is sent from the automatic sample measuring device 2 to the mixing tank 3, so that the liquid sample is mixed with the liquid sample in the mixing tank 3 and colored. Therefore, the degree of coloring of the colored liquid sample is measured by a colorimeter 4 to 100% in pure water.
Measure and record in comparison to transmittance.

〔Example〕

Hereinafter, embodiments of the apparatus of the present invention will be described with reference to the drawings, and reference will be made to embodiments of various coloring tests.

FIG. 2 shows an automatic coloring test apparatus used for experiments in a laboratory or the like.

First, a housing whose inside is heated to a predetermined temperature
Inside 10, a sample container 11 containing a liquid sample is provided. An air cylinder device 12 is provided on the top plate of the housing 10 corresponding to the upper part of the mouth of the sample container 11. The piston rod of the air cylinder device 12 can move forward and backward toward the mouth of the sample container 11, and a nozzle 13 for sucking a liquid sample is attached to the piston rod. The nozzle 13 is connected by a flexible tube to a negative pressure source 14 via a measuring container 21 forming the automatic sample measuring device 1, and the negative pressure of the negative pressure source 14
The sample inside is sucked into the measuring container 21.

As shown in FIG. 3, the measuring vessel 21 surrounds an intermediate portion of the main measuring pipe 22 extending in the vertical direction with an outer pipe 23, and allows nitrogen gas at a predetermined temperature (45 ° C.) to pass through the outer pipe 23. Thereby, the liquid sample in the main measurement pipe 22 is maintained at the temperature of the nitrogen gas, the lower end of the main measurement pipe 22 is connected to the nozzle 13 via an automatic valve 24, and the upper end is provided via an automatic valve 25. And is selectively connected to the negative pressure source 14 and the pressurized gas source 26.
When the negative pressure source 14 is selected, the liquid sample is sucked into the main measuring pipe 22 at a negative pressure, and the pressurized gas source 26 is selected after the measurement. To extrude. Here, the gas used for the pressurized gas source 26 is preferably an inert gas so as not to affect the liquid sample, and here, a nitrogen gas having a pressure of 0.5 kgf / cm ² G was used.

A light source switch 27 for detecting the liquid level is provided at the upper end of the main measuring pipe 22. The light source switch 27 is provided with a light-emitting portion and a light-receiving portion facing each other with the main metering tube 22 interposed therebetween. When the liquid surface of the liquid sample rises in this portion, the liquid surface is moved from the light-emitting portion to the light source. When the light is disturbed, the output voltage from the light receiving unit fluctuates to be turned on, thereby detecting the liquid level. Also, the lower end of the measuring main pipe 22 is
It is connected to the mixing tank 3 via automatic valves 24 and 28.

As shown in FIG. 4, the mixing tank 3 is a double container, and a nitrogen gas at a predetermined temperature (45 ° C.) between the inner container 41 and the outer container 42 is sequentially supplied. The liquid sample inside is kept at the predetermined temperature (45 ° C.).

Further, three injection pipes 43, 44, 45 are connected to the upper part of the inner container 41, and one of the injection pipes 43 is connected to the automatic valves 33, 34 and the deaeration tank 31 via pure water. Container 32 is connected,
When the automatic valves 33 and 34 are opened, the pure water in the pure water container 32 is deaerated in the deaeration tank 31 and sucked into the mixing tank 3 by the negative pressure of the negative pressure source 14. .

When pure water at normal temperature is directly supplied to the flow path of the heating atmosphere,
Colorimeter 4 to generate bubbles due to release of dissolved air
Therefore, the pure water is kept at the system temperature for a certain period of time in the deaeration tank 31 because it is not possible to adjust the indicated value to the correct 100% scale.

Further, another injection pipe 44 provided at the upper part of the inner container 41 is connected to a connection pipe between the nozzle 13 and the main measurement pipe 22 through the automatic valve 24, and further, another injection pipe 44 is provided. A pipe 45 is connected to the automatic reagent meter 2 via an automatic valve 56.

The automatic reagent measuring device 2 includes a measuring tube 51 and a coloring reagent container.
The measuring tube 51 is formed by winding a tube of a predetermined length, and is connected to a coloring reagent container 52 by a circulation line 53, and the liquid coloring reagent in the container 52 is naturally dropped. Is circulated through the measuring tube 51, and the photoelectric switch 54 at the upper end of the measuring tube detects the liquid level of the coloring reagent in the tube to perform measurement.

Then, by the pressurized nitrogen from the pressurized gas source 26 connected to the measuring pipe 51 via the automatic valve 55, the reagent in the measuring pipe 51 is fed into the mixing tank 3 via the automatic valve 56. Has become.

On the other hand, an iron piece 61 wrapped in a corrosion-resistant resin as a rotor of a magnetic body is freely movably accommodated in a bottom portion of the inner container 41 of the mixing tank 3. A magnetic stirrer (trade name) 62 is provided below the mixing tank 3 as a stirrer for rotating the iron piece 61.

Note that, instead of the iron piece 61, a stirring blade is rotatably provided on the inner bottom of the inner container 41, and a rotating blade is provided between the bottom of the inner container 41 and the bottom of the outer container 42. Are connected by a shaft, and the rotating blades are rotated by a nitrogen gas flow sent between the inner container 41 and the outer container 42, so that an air motor type stirring system in which stirring is performed by the stirring blades may be employed.

In the mixing tank 3, a discharge pipe 46 for discharging a colored liquid sample is connected to the bottom of the inner container 41, and the discharge pipe 46 is connected to a waste liquid container 85. Further, a photoelectric switch 47 including a light emitting unit and a light receiving unit is provided with the discharge tube 46 interposed therebetween, and the completion of discharge of the liquid sample is detected by the photoelectric switch 47.

Here, the colorimeter 4 is of a photoelectric type, and as shown in FIG. 5, a light source (single light beam) 71, an aperture 72, a lens 73, an interference filter 74, a cell 75, a lens 76, a shutter 77, a light receiving The elements 78 are arranged in a line, and the light emitted from the light source 71 and passing through the cell 75 is received by the light receiving element 78, photoelectrically converted, the current is amplified by the amplifier 79, and the needle of the transmittance indicating meter 80 is shaken. It is to let. To calibrate the colorimeter 4, the pure water was
This is done by adjusting the indicated value of the needle when introduced to the scale of 100%.

The cell 75 is of a flow cell type capable of measuring the light transmittance while the liquid sample is flowing without being stored.

The liquid sample that has passed through the cell 75 is then
It is discharged to 85 and further discharged to a waste liquid tank 86.

However, in the chemical coloring test apparatus of the present invention, the cell 75 of the colorimeter 4 and the mixing tank 3 are integrally formed, and the mixing tank 3 also serves as the cell 75. It has a function as a cell 75 of the color meter 4. To elaborate,
As shown in FIG. 6, a pair of optical fibers 87 and 88 are provided in the inner container 41 of the mixing tank 3 so as to face each other, and a light source (single light beam) 71, a diaphragm 72, a lens 73, and an interference filter 74 are provided. ,
The cell 75 (the optical fiber 87, the inner container 41 of the mixing tank 3, the optical fiber 88), the lens 76, the shutter 77, and the light receiving element 78 are arranged in a line. The colorimetric test by the colorimeter 4 is performed in the mixing tank 3, that is, the cell 75, without moving the colored liquid sample in the mixing tank 3 from the mixing tank 3.

An operation control unit 5 for controlling the operation of each unit described above is provided. The operation control unit 5 is based on a so-called microcomputer, and controls a series of operations from the supply of the sample to the measurement by the colorimeter 4 and the discharge, and the accompanying operations.

In FIG. 2, reference numeral 91 denotes a pressure regulator for heating nitrogen gas through which nitrogen gas at 3 kgf / cm ² G and 45 ° C. is supplied for heating. Reference numeral 92 denotes a pressure regulator for the pressurized gas source 26, through which 0.5 kgf / cm ² G of nitrogen gas is supplied for pumping. Reference numeral 93 denotes an overflow container that receives the mixed liquid when the liquid overflows from the mixing tank 3.

When the present apparatus is used in a chemical plant, the main measuring pipe 22 of the automatic sample measuring instrument 1 is connected to a production line.

Next, an operation example based on microcomputer control of this device will be described.

First, the pure water in the pure water container 32 is deaerated in the deaeration tank 31,
It is sent to the mixing tank 3, passes through the cell 75 of the colorimeter 4, passes through the waste liquid container 85, and is discarded in the waste liquid tank 86. During this time, the inside of the inner vessel 41 of the mixing tank 3 or the inside of the pipeline connecting the respective parts is washed with pure water, and the calibration of the colorimeter 4 with pure water is performed.

Next, by the same operation as the main measurement described below, the liquid sample is sequentially passed through the measuring main pipe 22, the mixing tank 3, that is, the cell 75 of the colorimeter 4, and the respective parts are washed together.

After pre-washing, start the main measurement. Hereinafter, the main measurement will be described.

First, the air cylinder device 12 is operated based on the measurement command, and the nozzle 13 is lowered together with the piston rod, and the tip is inserted into the liquid sample in the sample container 11.

Then, the liquid sample in the sample container 11 is sucked into the main measuring pipe 22 of the automatic sample measuring device 1 by the negative pressure of the negative pressure source 14. When the liquid level of the liquid sample in the main measuring pipe 22 rises to the position of the photoelectric switch 27, the connection between the main measuring pipe 22 and the negative pressure source 14 is cut off, and then the connection between the main measuring pipe 22 and the pressurized gas source 26 is performed. , And the liquid sample in the main measuring pipe 22 is fed into the mixing tank 3 under pressure.

In the mixing tank 3, since the heated nitrogen flows between the outer container 42 and the inner container 41, the liquid sample in the inner container 41 is heated and maintained at a predetermined temperature (45 ° C.). Then, a predetermined amount of the coloring reagent measured is sent from the automatic reagent measuring device 2 into the inner container 41 of the mixing tank 3 under pressure, so that the liquid sample and the coloring reagent are mixed in the inner container 41. I do. Then, the stirrer 62 is operated, and the rotation of the rotor 61 stirs and mixes the liquid sample and the coloring reagent.

When the mixing is completed, the mixture is allowed to stand for a certain period of time, and after defoaming, the liquid sample colored by mixing with the coloring reagent is kept in the mixing tank 3 also serving as the cell 75 of the colorimeter 4. ,
The degree of coloring is measured with a colorimeter 4. By the way, depending on the type of the coloring test, the degree of coloring changes with time, so that quick measurement is required. However, in the test apparatus of the present invention, since the mixing tank 3 is integrated with the cell 75 and is also used, it is configured. In addition, the measurement can be performed immediately after mixing, and a highly reliable and accurate measurement result can be obtained.

When the measurement is completed, the liquid in the mixing tank 3 is expelled into the waste liquid container 85 and discarded. The waste liquid in the waste liquid container 85 is transferred to the waste liquid tank 86 under the natural flow, and then processed.

<Test Example 1> Hereinafter, a case where a sulfuric acid coloring test of phenol was performed using this apparatus will be described.

In this test method, molten phenol and concentrated sulfuric acid are mixed in equal volumes, and the coloring degree of the obtained mixture is measured under a light wavelength of 532 nm.
It is indicated by the transmittance measured using a cell having an optical path length of 20 mm.

In this test, the mixing involves a temperature rise of about 75 ° C., which is extremely dangerous. In addition, since the viscosity of the mixed liquid increases, the liquid unevenness when transferring to the cell of the colorimeter 4 in the conventional method is used. However, there are drawbacks such as that this causes variation in transmittance measurement.

Therefore, the inner container 41 is used by using the double mixing tank 3 described above.
While flowing nitrogen gas at 45 ° C. at a rate of 30 (l) per minute between the inner container 41 and the outer container 42, 20 ml of concentrated sulfuric acid was added to the molten phenol in the inner container 41 over 3 minutes. There was no variation in the measurement results, and a result equivalent to the data of the test in the conventional method was obtained. FIG. 6 shows the comparison data.

Since the sample has a freezing point of about 41 ° C,
Kept.

<Example 2> Next, a sulfuric acid coloring test of glycol was performed with the present apparatus.

In this test, 5 ml of a concentrated sulfuric acid at room temperature was added to 5 ml of a sample kept at 10 ± 0.5 ° C., mixed, cooled again to 10 ± 0.5 ° C., and the transmittance at 390 nm was measured.

In the automation of this test method, the following points are devised.

To improve the measurement accuracy of samples and reagents,
It was increased from 5 ml to 10 ml.

Although the temperature before the test was specified as 10 ± 0.5 ° C, the temperature of the reagent was not specified as it was at room temperature, but it was necessary to cover the worsening of the heat release due to the doubling of the mixing volume. In order to make the final mixing temperature the same level as in the manual analysis, both the sample and the reagent were also kept at 15 ± 1 ° C.

The mixture was specified to return to 10 ± 0.5 ° C. Under these conditions, however, the viscosity would increase and it would be difficult to transfer the colorimeter to the 4 cell unit. Since this was not preferable, it was transferred to 4 parts of the colorimeter at 60 ° C. for measurement, and the transmittance value was corrected using the expansion coefficient.

<Test Example 3> Finally, an example in which a sulfuric acid coloring test of an aromatic hydrocarbon was performed by the present apparatus will be described.

In this test, concentrated sulfuric acid is added to a sample, mixed vigorously, and the degree of coloring of the obtained sulfuric acid layer is visually compared with a standard coloring liquid.

In the automation of this test method, the following points are devised.

The stirring for mixing is performed using an air motor, and the rotation speed of about 1500 rpm is maintained for 25 to 30 seconds by a stirring blade.

The inner container 41 of the mixing tank 3 was deepened so that the upper part of the container was three times the depth of night. With this device, dirt due to splashing during strong stirring can be prevented as much as possible.

After mixing, the liquid is separated into two layers, so that only the lower layer of sulfuric acid is led to the colorimeter 4, the arrival of the oil layer is detected by the photoelectric switch provided at the outlet of the mixing tank 3, and the transfer is stopped.

〔The invention's effect〕

By automating from the manual analysis, the reproducibility of the operating conditions was dramatically improved, and the measurement variation was reduced.

For example, in the phenol sulfuric acid coloring test, the standard deviation of manual analysis is about 1% for a sample with a normal transmittance level of 90%.
In contrast, the standard deviation was improved to 0.3% in the automatic device.

In addition, since the mixing tank and the colorimeter (cell) of the colorimeter are integrated and used, the degree of coloring can be measured quickly in the mixing tank for the liquid sample mixed and colored in the mixing tank. Can be. That is, since it is not necessary to transfer the liquid sample from the mixing tank to the colorimetric part (cell), the time required for the measurement can be reduced, and the coloring test can be performed quickly. As a result, it is possible to accurately measure the degree of coloring, which has conventionally been considered difficult to measure accurately because it changes with time, and to improve the reliability of the test.

Further, by integrating the mixing tank and the colorimeter (cell) of the colorimeter, the apparatus can be downsized and the automation of the apparatus can be facilitated.

Further, in this coloring test apparatus, before performing the coloring degree test on the sample, the colorimeter is calibrated using pure water supplied from the pure water supply unit to the mixing tank (that is, the cell of the colorimeter). Therefore, the accuracy of measurement of the degree of coloring of the sample performed thereafter is improved.

Further, since the mixing tank has an injection pipe connected to the automatic sample measuring instrument, an injection pipe connected to the automatic reagent measuring instrument, and an injection pipe connected to the pure water supply section, the sample, The reagent and the pure water can be reliably introduced into the mixing tank, and these liquids can be prevented from being scattered outside the mixing tank, so that the area around the mixing tank is not stained. Especially,
Although sulfuric acid is used as a reagent in this coloring test apparatus,
Since the mixing tank is provided with the injection pipe connected to the automatic reagent measuring instrument, sulfuric acid can be safely introduced into the mixing tank.

Further, since the mixing tank is provided not only with the above three injection pipes but also with a discharge pipe, the test liquid after the coloring test is quickly discharged from the mixing tank (that is, the cell of the colorimeter). This makes it possible to quickly prepare for the next coloring test and to facilitate the automation of the device.

When this coloring test apparatus is used in a production line, the quality of the product can be improved and the yield can be improved by feeding back the test results to the production line.

As a result, it becomes possible to finely clarify the factors related to the operation control of chemical manufacturing equipment, and contribute to the establishment of stable operation conditions,
This has made it easier to control product quality.

The automation reduced the personnel load and danger associated with sampling, minimized the time loss until the measurement results were obtained, and contributed to the improvement of speed. In addition, there was no danger during manual analysis due to unattended operation.

[Brief description of the drawings]

FIG. 1 is a schematic view showing an example of the apparatus of the present invention, FIG. 2 is a detailed view thereof, FIG. 3 is a view showing an example of an automatic sample measuring device, and FIG. 4 is an example of a mixing tank. FIG. 5 is a schematic diagram showing an example of a colorimeter, and FIG. 6 is a graph showing comparison data between a conventional method value and a measurement value of an automatic apparatus according to the present invention in a sulfuric acid coloring test of phenol. . 1 ... automatic sample measuring device, 2 ... automatic reagent measuring device, 3 ...
Mixing tank, 4 ... Colorimeter, 5 ... Operation control unit, 6 ... Pure water supply unit, 43,44,45 ... Injection pipe, 46 ... Discharge pipe, 75 ... Cell.

 ──────────────────────────────────────────────────続 き Continuation of the front page (72) Nobuo Horiji, Inventor No. 3, Chigusa Beach, Ichihara-shi, Chiba Mitsui Petrochemical Industry Co., Ltd. (56) References JP-A-57-119257 (JP, A) JP-A-60 JP-A-73438 (JP, A) JP-A-61-215950 (JP, A) JP-A-56-168148 (JP, A) JP-A-57-171266 (JP, A) )

Claims (1)

(57) [Claims] An automatic sample measuring device for measuring a liquid sample such as phenol, glycol or aromatic hydrocarbon, and an automatic reagent measuring device for measuring sulfuric acid as a coloring reagent.
A pure water supply unit 6 for supplying pure water; an injection tube 44 connected to the automatic sample measuring device 1; an injection tube 45 connected to the automatic reagent measuring device 2;
A mixing tank 3 having an inlet pipe 43 and an outlet pipe 46 connected to the liquid tank and mixing the liquid sample and the coloring reagent; and the mixing tank 3 serving as a cell 75, and the degree of coloring of the liquid in the mixing tank 3 The operation control unit 5 includes: a pure water supply unit 6 for introducing pure water into the mixing tank 3; and a colorimeter using the pure water. Calibrate 4 and
After the calibration, the pure water is discharged from the discharge pipe 46, and then the liquid sample is introduced into the mixing tank 3 from the automatic sample measuring device 1.
The coloring reagent is introduced from the automatic reagent measuring device 2 into the mixing tank 3,
An automatic chemical coloring tester configured to measure the degree of coloring with the colorimeter 4 after the coloring reaction is completed.