JPS63109355A - Method and apparatus for automatic distillation test - Google Patents

Abstract

PURPOSE:To accurately perform an automatic distillation test, by purging the distillate of the petroleum product in a measuring instrument with gas after the finish of measurement. CONSTITUTION:When measurement is finished, a signal is sent to the third solenoid valve 33 from a computer (CPU) 12 and the opening and closing valve 16 of a discharge pipe is opened by the valve 33 and the opening and closing valve 31 of a pressure control pipe is closed. Thereafter, the opening and closing valve 27 of a gas flow pipe is opened upon the reception of the signal from CPU 12 and nitrogen gas flows through the gas flow passage 29 to be blown in the second specimen supply pipe 5 and a detection pipe 10 and the distillate remaining in the measuring instrument of the pipe 10 is purged to be perfectly discharged in a distillate discharge part 18. When the purging due to the nitrogen gas is finished, the valve 33 is operated by the signal from CPU 12 and the valve 16 is closed and the valve 31 is opened. By this operation, the pressure remaining in the pipe 10 becomes equal to atmospheric pressure at the time of the purging due to the nitrogen gas. By this method, since the distillate remaining in the instrument 15 can be perfectly purged by the nitrogen gas, an accurate distillation property is always obtained.

Description

[Detailed Description of the Invention] [Industrial Application Field] The present invention provides an automatic method for measuring the distillation properties of petroleum products.
J Distillation Test Method and Apparatus.

[Background technology and its problems]

Distillation tests have been conventionally performed to measure the distillation properties of petroleum products such as gasoline, aviation fuel, kerosene, light oil, heavy oil, lubricating oil, and the like.

Such distillation tests have conventionally been carried out using the apparatus shown in FIG. In FIG. 2, the sample collection section 5
A sample of a petroleum product such as light oil sent from 0 through a switching valve 51 is measured in a measuring cup 52 and then injected into a flask 55 through a sample supply pipe 54 equipped with a switching valve 53. The sample in the flask 55 is heated by the heater 56, and a portion of the sample evaporates and reaches the cooling pipe 57, where it is liquefied and dripped as a distillate into the detection tube within 5 days for distillation. The amount of distillate being distilled is detected by a liquid amount detector 59, the distillation temperature is detected by a thermocouple 60, and the distillate is sent to the CPU internal circuit via a converter such as a V/I converter 61. is input into the computer 62 of. As the distillation progresses and the level of the distillate in the detection tube rises within 5 days and reaches a preset distillation point, the computer 62 stores the distillation amount and distillation temperature at that time. The distillation point is usually 225 according to JIS standard.
4. When the distillation is completed, heating by the heater 56 is stopped, the switching valve 53 of the sample supply pipe 54 and the switching valve 64 provided in the middle of the distillate discharge pipe 63 are opened, and the distillate is discharged from the detection pipe 58. Distillate is discharged to a distillate discharge section 65 via a discharge pipe 63. Reference numerals 66, 67, and 68 in FIG. 2 are solenoid valves, and these solenoid valves 66 to 6 operate the switching valves 51, 53, and 64, respectively, in response to signals from the computer 62. It has become.

However, in such a conventional example, the distillate in the detection tube 58 is discharged by opening the switching valves 53 and 64 as described above.
This is done by natural outflow due to atmospheric pressure, so if the viscosity is high, the distillate may remain in the measuring instrument or adhere to the wall of the measuring instrument and will not be completely discharged.
If the distillate remains in the tank and you start measuring the distillation properties in that state, the sum of the remaining liquid volume and the true distilled volume will be detected as the actual distilled volume, so it will be accurate. There is a problem in that it is not possible to measure the distillation properties.

[Object of the Invention] An object of the present invention is to provide an automatic distillation test method and apparatus that allow accurate testing.

Means and operation for solving problem C] The automatic distillation test method of the present invention is to remove the distillate remaining in the measuring instrument such as the detection tube or flask or attached to the wall after the measurement is completed by nitrogen gas. It is purged with gas such as Thereby, no distillate remains in the measuring instrument, and the measurement can always be started from a zero state with no remaining distillate, thereby achieving the above object.

The automatic distillation test device of the present invention is provided with a gas flow path that is connected to the upstream side of the distillate discharge pipe of a measuring instrument equipped with a distillate discharge pipe and that allows gas to flow through the gas flow path. A gas flow path opening/closing valve is installed in the middle of the gas flow path, and a gas supply source is connected to the gas flow path.When the gas flow path opening/closing valve is opened, the gas flows from the gas supply source into the measuring instrument via the gas flow path. A gas is supplied which aims to achieve this purpose by purging the distillate in the measuring device.

〔Example〕

Hereinafter, one embodiment of the present invention will be described based on the drawings.

FIG. 1 shows a schematic configuration of an embodiment of an automatic distillation test apparatus according to the present invention.

In FIG. 1, the automatic distillation test apparatus is equipped with a sample collection section 1 for collecting a predetermined amount of a sample of petroleum products such as light oil, and this collection section 1 has a first switching valve 2 equipped with a first switching valve 2 in the middle.
A sample supply tube 3 is connected. This first sample supply tube 3
On the downstream side, there is a second measuring cup with a measuring cup 4 at one upstream end.
A sample supply pipe 5 is connected, and this second sample supply pipe 5 is provided with a second switching valve 6 in the middle, and the other downstream end thereof is connected to a flask 7 as a heating container. One end of the first gas flow pipe 20 having a first solenoid valve 19 in the middle is connected to the operating part 2A of the first switching valve 2, and one end of the first gas distribution pipe 20 has a second solenoid valve in the middle to the operating part 6A of the second switching valve 6. One end of a second gas flow pipe 22 having a second gas flow pipe 21 is connected to the second gas flow pipe 22 . The other ends of these first and second gas flow pipes 20.22 are
They are joined together and connected to one end of the gas distribution main pipe 23. This gas distribution main pipe 23 has a regulator 24 in the middle for supplying nitrogen gas at a predetermined pressure, and the other end is connected to a gas supply source 25 such as a gas cylinder. Here, the first and second solenoid valves 19.2
1 is connected to a computer 12 in the CPU, and is opened and closed in response to a signal according to a sequence from the computer 12. As a result, the sample taken in the sample collection section 1 is transferred to the first switching valve 2 when the first switching valve 2 is opened. Then, when the first switching valve 2 is closed and the second switching valve 6 is opened, the sample in the measuring cup 4 is injected into the flask 7. It looks like this.

A heater 8 connected to a computer 12 is provided at the bottom of the flask 7, while one end of a cooling tube 9 is connected to the top of the flask 7, and a detection tube 1 is connected to the other end of the cooling tube 9.
The sample in the flask 7 is heated by the operation of the heater 8, and the vapor generated by the heating is liquefied in the cooling tube 9 and dripped into the detection tube 10 as a distillate. has been done. The level gauge IOA of the detection tube 10 is provided with a liquid amount detector 11 composed of, for example, one or more photocouplers, in order to measure the distilled amount, and this liquid amount detector 11 is connected to a computer 12. The amount of distillate dropped into the detection tube 10 is sent to the computer 12, and thereby the amount of distillate is measured discontinuously. Further, a thermocouple 13 for detecting the distillation temperature is provided in the cooling pipe 9, and this thermocouple 13
It is connected to a V/I converter 14 that converts the voltage signal sent from the thermocouple 13 into a current signal. It is made possible to do so. At this time, the computer 12 stores all the distillation amounts measured by the liquid amount detector 11, and when the distillation amount reaches a preset amount, the computer 12 changes the set temperature at that time to the distillation amount. The distillation temperature is stored separately as the distillation temperature, and the distillation amount and distillation temperature are output during the measurement or when the measurement is completed. Furthermore, since all measured values such as distillation amount and distillation temperature are stored in the computer 12, they can be re-outputted later as needed, and appropriate corrections can be made. Here, a measuring instrument 15 includes a flask 7, a cooling tube 9, and a detection tube 10.

At the bottom of the detection tube 10, there is a discharge pipe opening/closing valve 1 in the middle.
6 is connected to the distillate discharge pipe 17, and the second discharge pipe 1
A distillate discharge part 1 is provided below the detection tube 11, through which the distillate in the detection tube 11 is discharged.

A fourth gas distribution pipe 26 is connected to the main gas distribution pipe 23, and the fourth gas distribution pipe 26 includes a solenoid valve that performs predetermined opening and closing operations in response to a signal from the computer 12. A gas passage opening/closing valve 27 is provided, and a regulator 28 is further provided on the downstream side thereof. Further, this fourth gas distribution pipe 26 is branched into two branch pipes 2.6A and 26B on the downstream side of the regulator 28, and the second branch pipe 26A is the second switching valve of the second sample supply pipe 5. 6, the other branch pipes 26B are connected to the top side of the detection tube 10, and nitrogen gas is blown into these to purge the distillate in the measuring instrument 15 for a predetermined period of time, for example, about 5 minutes. It looks like this. Here, the gas flow path 29 includes the gas flow main pipe 23, the fourth flow pipe 262, and the branch pipes 26A and 26B.

One end of a pressure adjustment pipe 30 is connected to the middle of the other branch pipe 26B in the gas flow path 29, and this pressure adjustment pipe 30
A pressure regulating tube opening/closing valve 31 is provided in the middle, and the other end is opened to the distillate discharge part 18, so that when this valve 31 is opened, the pressure inside the detection tube 10 becomes equal to atmospheric pressure. There is. The pressure regulating pipe opening/closing valve 3
A third gas distribution pipe 32 is connected to the operation section 31A of the first valve and the operation section 16A of the discharge pipe opening/closing valve 16, and the third gas distribution pipe 32 is provided with a third solenoid valve 33 in the middle. , is connected to the middle of the fourth gas distribution pipe 26. The third solenoid valve 33 receives a signal from the computer 12 and opens the discharge pipe opening/closing valve 16 and closes the pressure regulating pipe opening/closing valve 31 when the distillation measurement with the measuring instrument 15 is completed. Further, when the purging of the measuring instrument 15 and the like with nitrogen gas is completed, the discharge pipe opening/closing valve 16 is closed and the pressure regulating pipe opening/closing valve 31 is opened.

Next, an example of the automatic distillation test method according to the present invention will be described.

First, to perform a measurement, a sample is injected into the flask 7 by operating the sample sampling section 1 and the first and second switching valves 2.6. Thereafter, when the sample in the flask 7 is heated by the heater 8, the sample is distilled, and the distillation properties are measured by a detector IO or the like.

By this measurement, most of the sample in the flask evaporates and is distilled into the detection tube 10 as a distillate, while a small portion remains in the flask 7 without evaporating or remains in the cooling tube 9.
Adheres to walls such as At this time, since the pressure adjustment tube opening/closing valve 31 is open, the pressure inside the detection tube 10 is maintained at atmospheric pressure, and pressurized distillation is prevented.

When the measurement is completed, the third W magnetic valve 3 is sent from the computer 12.
3, the third solenoid valve 33 opens the discharge pipe opening/closing valve 16 and closes the pressure regulating pipe opening/closing valve 31.

Thereafter, the gas flow path opening/closing valve 27 is opened in response to a signal from the computer 12, and nitrogen gas flows through the gas flow path 29 and is blown into the second sample supply tube 5, the detection tube 10, and the like. The distillate remaining in the measuring instrument 15 or adhering to the wall is purged and completely discharged to the distillate discharge part in one day. At this time, the second sample supply tube 5, the level gauge glass IOA of the detection tube 10, the distillate discharge tube 17, etc. are also purged, and dirt caused by carbon etc. caused by tar etc. accumulated in these is also removed. . Purging with nitrogen gas is performed for about 5 minutes, and upon receiving a signal from the computer 12, the gas passage opening/closing valve 27 is closed and the purging ends.

When the nitrogen gas purge is finished, the computer 12
In response to the signal, the third solenoid valve 33 is activated, the discharge pipe opening/closing valve 16 is closed, and the pressure regulating pipe opening/closing valve 31 is opened.

As a result, the pressure remaining in the detection tube 10 and the like during purging with nitrogen gas becomes equal to atmospheric pressure.

According to this embodiment, the distillate remaining in the measuring instrument 15 such as the detection tube 10 or attached to the wall can be purged and completely discharged even if the viscosity is high, using nitrogen gas. Therefore, measurements can always be started from zero and accurate distillation properties can be obtained.

Moreover, since it also serves as a purge for the lines such as the second sample supply pipe 5 and the distillate discharge pipe 17, it is possible to prevent the lines from being clogged with garbon or the like. Furthermore, the level gauge IOA of the detection tube 10 is also purged and cleaned, and malfunctions due to dirt are eliminated since the level gauge IOA is above 0, so the trouble of cleaning the measuring instrument 15 etc. is saved and the operating rate of the device is increased.
Since there are no errors in measurement, the reliability of the test has increased from 70% to 98%. Furthermore, in this embodiment, nitrogen gas is blown from two locations, the second sample supply tube 5 and the detection tube 10, so that the distillate remaining in the measuring instrument 15 or attached to the wall is sufficiently removed. Can be purged. Furthermore, since the distillate is purged with nitrogen gas, which is an inert gas, it is possible to prevent the measuring instrument 15 from exploding, and since the cost of nitrogen gas is relatively low compared to other inert gases, the distillate can be purged at low cost. Furthermore, the first and second switching valves 2.
6. Since the discharge pipe opening/closing valve 16 and purging of the distillate are performed using nitrogen gas supplied from the same gas supply source, the piping structure is simplified. In addition, since the third electromagnetic valve 33 is configured to open and close the pressure adjustment pipe opening/closing valve 31 and the distillate discharge pipe opening/closing valve 16 in opposite directions, it is possible to purge the distillate in the measuring instrument 15 and to This allows smooth switching between removing the residual pressure of nitrogen gas in the measuring instrument 15 and removing it.

In the above embodiment, the distillate was purged with nitrogen gas, but in the present invention, this purging may be performed with other inert gas such as helium or argon, or with air. Although the operation of the first switching valve 2 and the like and the purging of the distillate were performed using nitrogen gas supplied from the same gas supply source, in the present invention, these are supplied from separate gas supply sources. You can. Furthermore, the test may be performed by manually opening and closing valves, etc., by an operator without using the computer 12. Furthermore, in this embodiment, the sample from the sample collection section 1 was once measured using the measuring cup 4 and then stored in the flask 7, but in the present invention, the sample is directly injected into the flask core without using a measuring cup. It may be. Furthermore, the fourth gas flow pipe 26 constituting the gas flow path 29 is branched in the middle, and the measuring instrument 15
The distillate was purged by supplying nitrogen gas from two locations, but in the present invention, gas may be supplied from one or more locations of the measuring instrument 15 if it is upstream from the distillate discharge pipe 17. It may be something that does.

Furthermore, when gas is supplied from multiple locations, the supply pressure may be changed as necessary to adjust the supply amount at each location. Although the pressure regulating pipe opening/closing valve 31 is opened and closed in conjunction with each other by reverse operation, in the present invention, separate flow pipes may be provided and the operations may be performed at staggered times. Furthermore, in the above embodiment, the distillation test was conducted at normal pressure, but in the present invention, a pressure reducing means 40 such as a vacuum pump is connected to the pressure regulating tube 30 as shown by the chain line in FIG. According to this test, the retention properties of high boiling point petroleum products such as heavy oil and lubricating oil can be measured even at low temperatures. Further, in the present invention, the measuring instrument 15, the heater 8,
The first to third electromagnetic valves 19°21.33, the gas passage opening/closing valve 27, the discharge pipe opening/closing valve 16, etc. may be provided within the measuring section frame. Furthermore, although the liquid amount detector 11 is one or more photocouplers or the like that measure the distillation amount discontinuously, it may be a capacitance type or the like that can continuously measure the distillation amount.

〔Effect of the invention〕

According to the present invention as described above, there is an effect that an automatic distillation test can be performed accurately.

[Brief explanation of the drawing]

FIG. 1 is a schematic diagram of an embodiment of a device according to the present invention, and FIG. 2 is a schematic diagram of a conventional device. 15... Measuring instrument, 16... Discharge pipe opening/closing valve, 1
7... Distillate discharge pipe, 25... Gas supply source, 27.
...Gas flow path opening/closing valve, 29...Gas flow path, 30.
...Pressure gII adjustment pipe, 31...Pressure adjustment pipe opening/closing valve.

Claims (4)

[Claims] (1) An automatic distillation test method for measuring the distillation properties of petroleum products, which comprises purging the distillate of the petroleum product in the measuring instrument with gas after the measurement is completed. (2) The automatic distillation test method according to claim 1, wherein the gas is nitrogen gas. (3) In an automatic distillation testing device for measuring the distillation properties of petroleum products, it is connected to the upstream side of the distillate discharge pipe of a measuring instrument equipped with a distillate discharge pipe and allows gas to flow through it. An automatic distillation test device comprising a gas flow path, a gas flow opening/closing valve provided in the middle of the gas flow path, and a gas supply source connected to the gas flow path. (4) In claim 3, a pressure regulating pipe is connected to the gas flow path downstream of the gas flow opening/closing valve, and the pressure regulating pipe is provided with a pressure regulating pipe opening/closing valve. . An automatic distillation test apparatus, characterized in that the distillate discharge pipe is provided with a discharge pipe opening/closing valve that opens and closes in the opposite direction to the pressure regulating pipe opening/closing valve.