JPH0545361Y2 - - Google Patents

Description

[Detailed description of the invention] [Industrial application field] This invention is used in oil analysis systems to analyze various gas components present in oil such as transformer oil and determine the degree of deterioration. Regarding medium gas degassing equipment.

[Conventional technology]

As transformer oil deteriorates, it begins to contain gases such as H ₂ and CO, but as the degree of deterioration progresses, the amount of these gases increases, and carbonization such as C ₂ H ₆ and C ₂ H ₄ occurs. The amount of hydrogen will also increase.

Conventionally, the method of examining the degree of deterioration of oil such as transformer oil is to reduce the pressure in a container containing the oil, degas the gas from the oil, and introduce the gas into a gas chromatograph. Devices for this purpose include a Trithierly extractor, a piston extractor, and a bellows extractor (see Denki Kyodo Kenkyu, Vol. 36, No. 1).

[Problem that the invention attempts to solve]

As mentioned above, in order to degas the gas in the oil, devices such as the Tritiery method and the piston method are used to reduce the pressure. In order to do this, large-scale equipment is required. Furthermore, it is not easy to operate when setting the sample oil, and care must be taken at all times to prevent oil from entering when introducing the degassed gas into the gas chromatograph. Therefore, since the device is quite expensive and complicated to operate, there is a great need for it, but its widespread use has been slow.

[Means for solving problems]

In order to solve the above-mentioned problems, this invention has a gas-in-oil deaerator that connects a deaeration tank equipped with a sample oil inlet, a heating part, and a purge gas inlet, and a reflux cooling pipe. A pump is disposed in a closed pipe line in which a gas outlet in the reflux cooling pipe is connected to the purge gas introduction part via a gas chromatograph and a valve, so that the gas passage is a closed system and the gas circulates. It is characterized by

[Effect]

Put oil in a deaeration tank, connect the inside of this deaeration tank to the gas outlet, reduce the pressure with a pump, and further heat the heating part.The gas in the oil will be degassed and come out, but at the same time the oil will also be removed. It comes out as a little steam. The gas is then introduced into the gas chromatograph from a gas outlet provided midway through the cooling tube, but the oil that has turned into vapor is cooled and becomes liquid and falls back into the oil. Therefore, only the sample gas in the oil is sent to the gas chromatograph and analyzed, making it possible to determine the degree of deterioration of the oil.

〔Example〕

Hereinafter, specific embodiments of this invention will be described with reference to the drawings.

1 in FIG. 1 is a gas-in-oil deaerator according to this invention. Reference numeral 2 denotes a deaeration tank, into which the sample oil is measured and operated visually, and is introduced through the sample inlet 2A in a manner that prevents air from entering. Reference numeral 3 denotes a cooling tank, and the cooling tank 3 has a double structure in which a tube formed by connecting a curved tube 32 and a vertical tube 33 is inserted into an outer tube 31. In the lower part of this cooling tank 3, an outer tube 31 and a curved tube 32 are tightly joined, and a space 3A between the outer tube 31, the curved tube 32, and the vertical tube 33 is sealed, and the vertical tube 33 is directed downward. It has been extended.
Further, the outer tube 31 of the cooling tank 3 is provided with a cooling liquid inlet 34 at the lower part and a cooling liquid outlet 35 at the upper part, and furthermore, on the opposite side near the cooling liquid inlet 34 at the lower part, a spherical shape is provided. A gas outlet 36 is provided which communicates with the gas chromatograph from the vertical pipe 33.

The lower part 3B of the cooling tank 3 is tightly connected to the upper part 2B of the deaeration tank 2 to prevent gas from leaking from inside the deaeration tank 2. It is designed so that it can reach into the sample oil placed in the container. That is, when oil is put into the degassing tank 2 and a pump 41 (described later) is driven to reduce the pressure inside the degassing tank 2 and heated by the heater 4, the gas in the oil is degassed and comes out, but at the same time, the oil also becomes a little steam. It grows old and comes out. Therefore, the bent pipe 32 is cooled in a cooling tank 3, and the gas is made to exit from a discharge port 36 provided in the middle of the vertical pipe 33, so that the oil is cooled and dropped into the original oil as a liquid.

Further, in this figure, 4 is a heater for heating the sample oil, and 5 is a porous body, for example, a glass filter of about 100 mesh, and this glass filter serves to separate the oil part and the gas part.
6 is a purge gas inlet, 7 is a discharge pipe for discharging used oil, and 8 is a drain. Reference numeral 41 denotes a pump for reducing the pressure in the degassing tank 2, sucking the generated sample gas through the outlet 36, and sending it to the gas chromatograph. The gas-in-oil deaerator 1 is connected to the purge gas introducing section 6 via a valve, a high-pressure resistance pipe (described later), etc., and constitutes a closed system reflux device.

FIG. 2 is a diagram showing an embodiment in which the gas-in-oil deaerator 1 is connected to an analysis system using a gas chromatograph. In this figure, 10 is a ten-way valve for sampling and precutting. 11 is a measuring tube for measuring the sample, 12 is a measuring tube for measuring the target components (H ₂ , O ₂ ,
N ₂ , CH ₄ , CO, CO ₂ , C ₂ H ₆ , C ₂ H _{4 ,} etc.) into the main column 14 (packing material is Porapak-N, 3φ x 1 m), 13 is the flow rate Chi York column (packing material is Porapak-N, 3φ x 2m) to prevent fluctuations, 14
is the main column (the packing material is Porapak-N,
3φ×1m) and the sample was exposed to H ₂ , O ₂ , N ₂ , CH ₄ ,
This column is used to separate CO, etc. into two groups, such as CO ₂ , C ₂ H ₆ , C ₂ H ₄ and hydrocarbons having 3 or more carbon atoms. 15 is a resistance column for matching the resistance with the pre-column 12 and the main column 14 (the packing material is Porapak-N, 3φ x 2m), 16 is a four-way valve for switching the flow path, and 17 is the main column (the packing material is Molecular sieves 5A, 3φ×2m)
It is a column for H ₂ , O ₂ , N ₂ , CH ₄ , and CO analysis. 18 is the main column (filling material is
Porapak-Q, 3φ×1m) and CO ₂ , C ₂ H ₆ ,
This column is for analyzing C ₂ H ₄ and hydrocarbons with 3 or more carbon atoms. 19 is a thermal conductivity detector, 20
is a small reactor, 21 is a hydrogen flame ionization detector, 2
3 is an empty column for elution time delay adjustment. Further, 22 is a dummy column that is the same as the pre-column 12, and 24 to 26 are pressure regulators. The components from the ten-way valve 10 to the pressure regulator 26 are internal components of the gas chromatograph.

Sampling is performed by introducing the sample into the pressure regulator 24, ten-way valve 10, metering tube 11, and precolumn 12 using a carrier gas, and switching the valves from the solid line to the dotted line. That is, precolumn 1
2, and when the target component is introduced, the ten-way valve 10 is switched from the solid line to the dotted line. Unnecessary components (hydrocarbons of _C4 or higher) in the pre-column 12 are discharged to the VENT via the York column 13.

The target components are sent to the main column 14, but H ₂ , O ₂ , N ₂ , CH ₄ , and CO in this column are sent to the four-way valve 1.
After entering the main column 17 via the dotted line 6, switch to the solid line at the right time. Then, the CO ₂ , C ₂ H ₆ , which remains in the main column 17,
C ₂ H ₄ and hydrocarbons having 3 or more carbon atoms enter the main column 18 . Next, the components separated in each of the main columns 17 and 18 are combined and enter a thermal conductivity detector 19. This thermal conductivity detector 19 detects inorganic components such as H ₂ , O ₂ , N ₂ , CO, and CO ₂ . When the concentration of CO and CO ₂ is low, CO converted to CH ₄ by the small reactor 20,
A hydrogen flame ionization detector 21 detects the CO ₂ component.

In order to stabilize the baseline of the chromatogram obtained by the above method, care must be taken not to fluctuate the flow rate of the carrier gas, but in order to do so, the flow rate of the carrier gas must be set as follows: Precolumn 12 = Dummy column 22, York column 13 = Main column 14 + Main Column 1
7. It is desirable that the resistance column 15 = pre-column 12 + main column 14.

Also, 42, 43, 44 and 45 are valves, 4
6 is a high resistance tube. As shown in the figure, the above-mentioned components are connected through predetermined pipe lines to form an analysis system.

Next, a method for analyzing gas components in oil using an analysis system using the gas-in-oil deaerator 1 according to this invention will be described.

First, N ₂ gas is introduced into the system and purged at the same time, that is, valves 43 and 44 are opened, valve 45 is closed, N ₂ gas is introduced through valve 43, and then purged.
3 to "close" and then valve 44 to "close".

Accurately measure 200 ml to 500 ml of oil from the sample oil inlet 2A and put it into the deaeration tank 2. The valve 45 is then "open".

The temperature of the oil put in the deaeration tank 2 is controlled by the heater 4.
The temperature inside the cooling tank 3 is raised (40°C to 70°C) to 5°C to 10°C. In this state, the pump 41 is continuously driven for a certain period of time to degas the gas component in the oil.

After the pump 41 is stopped, the valve 42 is closed, and the valve 44 is opened, sampling is performed using the gas sampling tank (not shown) of the gas chromatograph. In this way, a gas chromatogram as shown in FIG. 3 is obtained.

The oil is discharged from the discharge pipe 7 by keeping the valve 44 "closed" and opening the valve 43 and the tank 8 provided in the waste oil pipe 7 to introduce _N2 gas.

As shown in Figure 4, for example, focusing on H ₂ ,
From normal oil to abnormal oil where the degree of deterioration gradually increases depending on the number of years the oil has been used.
Measure the amount of H ₂ , obtain a standard calibration curve in advance, and determine a reference value for replacement. The degree of deterioration of the unknown oil is determined by comparing the measurement results with a standard calibration curve, and if the value exceeds the guideline value, the oil should be replaced.

The details of this invention are as described above, but in the above embodiment, when the gas-in-oil deaerator and the gas chromatograph are combined, the measuring tube 11 for measuring the degassed gas is There can be considerable differences in the amount of gas produced. Therefore, the measuring tube 11
should be replaced depending on the gas concentration in the oil.
In addition, in gas chromatographs, H ₂ , O ₂ , CH ₄ ,
CO, CO ₂ , C ₂ H ₆ , C ₂ H ₄ , C ₂ H ₂ , etc. were analyzed in one sampling, but if you want to limit the analysis to a specific component, you can remove the four-way valve 16 and use a simpler configuration. It's okay.

Note that this invention can also be used in a system that measures hydrocarbons of _C3 or higher and about _C5 .

[Effect of idea]

Since the gas-in-oil deaerator according to this invention has the above configuration, H ₂ , O ₂ , CH ₄ , CO, CO ₂ , C ₂ H ₆ , C ₂ H ₄ , Components such as are degassed by bubbling _N2 gas,
The amount can be measured. In addition, it is possible to easily know the degree of deterioration of transformer oil etc. at a relatively low cost. At the same time, these gases
Since the metering tube of the gas chromatograph is charged, it can be quantitatively introduced into the gas chromatograph. There is also no need to worry about oil getting into the measuring tube (not shown) or the like.

[Brief explanation of the drawing]

Figure 1 is a schematic diagram of the gas-in-oil deaerator according to this invention, Figure 2 is an example diagram of the gas-in-oil deaerator connected to an analysis system using a gas chromatograph, and Figure 3 is the invention. Gas chromatograph for analyzing gas components in oil by connecting the gas-in-oil degassing device to a gas chromatograph, No. 4
For example, the figure focuses on H ₂ and measures the amount of H ₂ from a normal oil to an abnormal oil whose degree of deterioration gradually increases depending on the number of years the oil has been used.
FIG. 2 is a diagram of a calibration curve that serves as a standard determined in advance. 1... Gas in oil deaerator, 2... Deaerator, 2A
...Sample oil introduction part, 2B...Deaeration tank upper part, 3
...Cooling tank, 3A...Cooling tank internal space, 3B...
Cooling tank lower part, 31...outer pipe, 32...bent pipe, 33
... straight pipe, 4 ... heater (heating section), 5 ... glass filter, 6 ... purge gas introduction section, 7 ... discharge pipe, 41 ... pump.

Claims (1)

[Scope of utility model registration request] A degassing tank equipped with a sample oil introduction part, a heating part, and a purge gas introduction part is connected to a reflux cooling pipe, and the purge gas is introduced through a gas outlet in the reflux cooling pipe through a gas chromatograph and a valve. 1. A gas-in-oil degassing device characterized in that a pump is disposed in a closed pipe connected to a gas-in-oil gas degassing device, and the gas passage is a closed system in which the gas circulates.