JP2001235403A - Apparatus for injecting sample oil for gas analysis in vial - Google Patents

Abstract

PROBLEM TO BE SOLVED: To enhance the analytic accuracy of an air-containing component such as O2 or N2 and to shorten the injection operation time of sample oil. SOLUTION: In an apparatus for injecting sample oil for gas analysis in a vial 1 constituted so that first and second needles 3, 4 are inserted in the gas sealing port 10 of the vial 1 and carrier gas is blown to the second needle 4 from the first needle 3 through the interior of the vial 1 and, thereafter, the sample oil collected in a syringe 11 is injected in the vial 1 from the first needle 3, the vial 1 is evacuated before the carrier gas is blown.

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

The present invention relates to an oil-filled electric device,
In order to analyze the gas dissolved in insulating oil such as oil immersion cable and oil immersion bushing by gas chromatograph, it relates to a device that injects the insulating oil into a vial as a sample oil for gas analysis. The present invention relates to a device for injecting a sample oil for gas analysis into a vial.

[0002]

2. Description of the Related Art Oil-filled electrical equipment such as transformers is
Insulating oil for the equipment to diagnose abnormalities and perform maintenance
Collected in a syringe as a sample oil, and even with the headspace method
The amount of each type of gas dissolved in the sample oil
Analyzes have been performed by matograph. Oiled
If the electrical equipment becomes abnormal, the local
Partial heat generation occurs. This heat causes insulation oil and
Various gases are generated due to thermal decomposition of edge paper, and most of them are
The components dissolve in the insulating oil. For that, O_Two, N _Two, H
_Two, CO, CO_Two, CH_Four, C_TwoH_Two, C_TwoH_Four, C_Two
H₆Many types of gas are analyzed and oil input
An abnormality diagnosis of the gas appliance has been performed. Among them, oil-filled electric machine
Examples of the gas which is remarkably generated at the time of abnormality of the vessel include, for example,
C_TwoH_Two, C_TwoH_FourIs mentioned. That is, C_TwoH_Two
Is a specific gas generated when a discharge occurs._Two
H_FourIs a special gas generated when discharge or overheating occurs.
is there. Therefore, any of these gases can be diagnosed as abnormal.
It is an important gas for performing. Electric cooperative research in Japan
In the diagnosis of oil-filled electrical equipment,_TwoH_Twoof
Caution level 0.5 ppm, C_TwoH_FourCaution level
Is set to 10 ppm. In addition, maintenance pipes for oil-filled electrical equipment
The important gas components in the process are O_Two, N _TwoSuch as
Air-containing components. For high voltage oil-filled electrical equipment
If air enters the insulating oil from outside, insulation problems may occur.
The title arises. In order to keep the insulation of insulating oil good, O_Two
And N_TwoIs dissolved in insulating oil at 0.5% to several% or less
It is necessary to have something.

FIG. 3 is a cross-sectional view for explaining the analysis principle of the headspace method.
(B) shows a state in which the vial 1 is heated and stirred. In FIG. 3A, a sample oil 2 collected by a syringe from an oil-filled electric device is stored in a vial 1, and a gas filling port 10 is sealed with a lid 17 with packing. The gas dissolution amount of the sample oil 2 is assumed was C _a. In the vial 1, a gas phase portion 2A is formed above the liquid sample oil 2. When the vial 1 is heated and stirred, the gas 2C dissolved in the sample oil 2 is extracted into the gas phase 2B as shown in FIG. here,
_Let the gas concentration of the liquid sample oil 2 be C _i , the gas concentration of the gas phase part 2B be C _g , and the distribution coefficient K be C _i / C
Define as _g . The headspace method utilizes the principle that the gas concentrations C _g and C _i in the vial 1 are in an equilibrium state depending on the distribution coefficient K of each type of gas component. Since the distribution coefficient K depends on the type and temperature of the gas, the gas concentration of the sample oil 2 in the gas concentration C _g in the gas phase portion 2B shown in FIG. 3 (A) at equilibrium C _a (Sample Oil 2
Gas dissolved amount). Therefore, gas analysis is performed by supplying the gas in the gas phase portion 2B in FIG. 3B to the gas chromatograph side. When performing gas analysis by this headspace method, it is necessary to inject the sample oil 2 previously collected by a syringe from the oil-filled electrical equipment into the vial 1 without touching the outside air.

FIG. 4 is a partially broken side view showing the configuration of a conventional apparatus for injecting a sample oil for gas analysis into a vial. That is, the upper side of the boundary 50 in FIG. 4 is a side view, and the lower side of the boundary 50 is a cross-sectional view in which the internal configuration can be seen. The first needle 3 and the second needle 3
Needle 4 is inserted. The upper end of the first needle 3 is connected to the three-way cock 8 and the lower end communicates with the inside of the vial 1. On the other hand, the upper end of the second needle 4 is open to the outside air and the lower end communicates with the inside of the vial 1. The three-way cock 8 is connected to the carrier gas supply device 6 via the gas flow meter 7 and the opening / closing valve 6A, and is also connected to the third needle 5 of the syringe 11. The internal pressing portion 12 of the syringe 11 is
3 and manual pusher 13 by hand 14
Can be pressed.

In FIG. 4, before the sample oil 2 in the syringe 11 is pushed out, the three-way cock 8 is set so that only the gas flow meter 7 and the first needle 3 communicate with each other.
Next, the opening / closing valve 6A is opened and the carrier gas supply device 6 is opened.
From the carrier gas such as Ar gas,
It flows into the vial 1 via the first needle 3 and is discharged to the outside air via the second needle 4. The blowing of the carrier gas drives off the residual air inside the vial 1. Next, the three-way cock 8 is set so that only the third needle 5 side and the first needle 3 side of the syringe 11 communicate with each other. Manual pusher 1 in that state
When sample 3 is pressed downward by hand 14, sample oil 2 flows into vial 1. After the oil supply to the vial 1 is completed, the first needle 3 and the second needle 4 are withdrawn, the vial 1 is set on a gas chromatograph (not shown), and gas analysis is performed.

[0006]

However, the conventional apparatus for injecting a sample oil for gas analysis into a vial as described above has a problem that the accuracy of gas analysis of air-containing components is low and the operation is time-consuming. . That is, in the conventional apparatus, since only the carrier gas is blown off, the rejection rate of the residual air in the vial is low, and the analysis accuracy of O ₂ and N ₂ which are the same kind of gas as the air dissolved in the sample oil is improved. Was bad. In addition, since the conventional apparatus is manually operated, the operation of injecting the sample oil requires a lot of time, and the analysis results also vary. The purpose of this invention, O ₂ and N
_The object of the present invention is to improve the analysis accuracy of air-containing components such as _2, and to shorten the injection time of sample oil.

[0007]

According to the present invention, there is provided an apparatus for injecting a sample oil into a vial for analyzing a gas dissolved in the sample oil, the apparatus comprising: The first needle and the second needle are inserted into the gas filling port of the vial, and the carrier gas is blown from the first needle through the vial to the second needle, and then the sample oil collected in the syringe is removed. In a device for injecting a sample oil for gas analysis, which is injected into the vial from the first needle, into the vial, the inside of the vial may be evacuated before the carrier gas is blown. As a result, air is almost completely removed from the vial by evacuation, so that the accuracy of analysis of air-containing components such as O ₂ and N ₂ in gas analysis is improved.

In this configuration, the step of evacuating the vial, the step of blowing carrier gas into the vial, and the step of injecting sample oil from the syringe into the vial are automatically operated. You may. As a result, the injection time of the sample oil is shorter than before. Further, in such a configuration, a valve head is provided in which first and second needles inserted into a gas filling port of the vial are projected downward, and a third needle from a syringe is inserted from above, A valve head communicates with the first check valve from the first needle to the evacuation device, a second check valve from the first needle to the carrier gas supply device, and a communication from the first needle to the third needle of the syringe. A third check valve; and a fourth check valve communicating from the second needle to the outside air. The first and second needles are inserted into the gas filling port of the vial by moving the valve head downward. You may make it become. As a result, the connection points of the pipes are collectively housed in the valve head, and the pipes are each provided with a check valve. Therefore, since there is no room for any components other than the sample oil to enter the vial side, the accuracy of gas analysis is further improved.

[0009]

DESCRIPTION OF THE PREFERRED EMBODIMENTS The present invention will be described below with reference to embodiments. FIG. 1 is a perspective view showing a configuration of an apparatus for injecting a sample oil for gas analysis into a vial according to an embodiment of the present invention, and FIG. 2 is a piping system diagram of FIG. The first needle 3 and the second needle 4 are connected to the gas filling port 1 of the vial 1.
It projects from the lower part of the valve head 16 so as to face zero, and is covered with a transparent safety cover 26. The third needle 5 of the syringe 11 is inserted into the upper part of the valve head 16. The syringe 11 has a receiving plate 34
And is connected to a manual handle 23 together with the valve head 16. Accordingly, the valve head 16 and the syringe 1 are operated by operating the manual handle 23.
1 moves up and down together. An internal pressing portion (not shown) of the syringe 11 is connected to an air cylinder 25 via a pusher 24. An air hose 27 is connected to the air cylinder 25, and high-pressure air 27 A from a high-pressure air supply device (not shown) flows in the direction of the arrow and is supplied to the air cylinder 25 via the air hose 27. A carrier gas pipe 29 is connected to the valve head 16 via a regulator 31, and a carrier gas 29 A, for example, Ar gas from a carrier gas supply device (not shown) is flowed in the direction of the arrow, and flows through the carrier gas pipe 29. And supplied to the regulator 31. The flow rate of the carrier gas 29 </ b> A is adjusted by the regulator 31 and supplied to the valve head 16.
Further, a vacuum pipe 28 is connected to the valve head 16,
A vacuum gauge 32 is attached to the vacuum pipe 28, and a vacuum exhaust device (not shown) is connected to the vacuum pipe 28 so that the air 28A in the valve head 16 is exhausted in the direction of the arrow.

In FIG. 2, as described above, the syringe 1 is inserted from above the container 16A of the valve head 16 (dotted frame).
One third needle 5 is inserted, and the first needle 3 and the second needle 4 protrude from the lower part of the container 16A. Inside the valve head 16, the upper end of the first needle 3
It is connected to a vacuum pipe 28 via a first check valve 18 and to a carrier gas pipe 29 via a second check valve 19. The upper end of the first needle 3 is also connected to the third needle 5 via the third check valve 20.
On the other hand, the upper end of the second needle 4 is connected via a fourth check valve 21 to an exhaust gas pipe 30 that communicates with the outside air. First
The needle 3 and the second needle 4 are arranged at positions below the valve head 16 so as to pierce the gas filling port 10 of the vial 1. The first check valve 18 allows the air 28A to flow only in the direction of the arrow (the exhaust side from the inside of the vial 1), and the second check valve 19 causes the carrier gas 29A to flow in the direction of the arrow (the supply into the vial 1). Side).
The third check valve 20 allows the sample oil 2 to flow only in the direction of the arrow (the supply side into the vial 1), and the fourth check valve 21 causes the carrier gas 29A to flow in the direction of the arrow (the vial 1).
It flows only to the exhaust side from inside). The air hose 27 is provided with a regulator 41 and an electromagnetic on-off valve 27B, and the carrier gas pipe 29 is provided with a regulator 31
And an electromagnetic opening / closing valve 29B. Further, a vacuum gauge 32 is attached to the vacuum pipe 28, and an electromagnetic on-off valve 28B is interposed. A vacuum exhaust device 36 is connected to an end of the vacuum pipe 28, and the carrier gas pipe 2
9 is connected to a carrier gas supply device 6. A high-pressure air supply device 37 is connected to an end of the air hose 27. The electromagnetic on-off valve 27B. 28
B and 29B can be automatically controlled by the control box 22 (FIG. 1).

Referring to FIGS. 1 and 2, the step of injecting the sample oil into the vial 1 will be described below. First, the syringe 11 from which the sample oil 2 has been collected is set on the receiving plate 34, and the third needle 5 is inserted into the container 16A of the valve head 16. Next, the sealing port 10 is sealed with the air still in the empty vial 1, and the vial 1 is set so as to be sandwiched by the clamp 1A. next,
When the manual handle 23 is lowered, the valve head 16 is lowered in conjunction therewith, and the first needle 3 and the second needle 4 are inserted into the filling port 10 of the vial 1. The above is the preparation step. The following steps are automatically controlled by the control box 22 and are executed continuously in the order of each step. In FIG. 2, first, starting from a vacuum exhaust step in the vial 1, the electromagnetic on-off valve 28 B of the vacuum pipe 28 is opened in a state where the electromagnetic on-off valve 27 B of the air hose 27 and the electromagnetic on-off valve 29 B of the carrier gas pipe 29 are closed. Then, the air 28A in the vial 1 is removed by the vacuum exhaust device 36, and the inside of the vial 1 is evacuated. In this state, the electromagnetic on-off valve 28B of the vacuum pipe 28 is closed, and the process of blowing carrier gas into the vial 1 is started. In this step, the electromagnetic on-off valve 29B of the carrier gas pipe 29 is opened, and the carrier gas 2 from the carrier gas supply device 6 is opened.
9A enters the vial 1 from the first needle 3, flows as shown by the arrow, is guided to the exhaust gas pipe 30 through the second needle 4, and is discharged to the outside air. Carrier gas 2 in vial 1
9A, the inside of the vial 1 is filled with only the carrier gas 29A. Finally, the electromagnetic on-off valve 29B of the carrier gas pipe 29 is closed, and the process of injecting the sample oil from the syringe 11 into the vial 1 is started. The electromagnetic open / close valve 27B of the air hose 27 is opened, and the high-pressure air 27A from the high-pressure air supply device 37 is sent to the air cylinder 25. Thereby, the air cylinder 25 operates and the pusher 24 is pressed downward, so that the sample oil 2 of the syringe 11 is pressed downward. For this purpose, the sample oil 2 is supplied to the vial 1 via the first needle 3.
It is injected into. The injection amount of the sample oil 2 in one operation of the syringe 11 can be preset by the adjustment knob 33 so as to be a fixed amount, for example, 15 ml.

In the above embodiment, since the air in the vial 1 is evacuated almost completely in advance by vacuum evacuation (the air rejection rate in the vial 1 is 99.99% or more), the air-containing component is 0.01% or less. And O ₂ in gas analysis
Analytical precision of air-containing components, such as and N ₂ are improved. As a result, the reliability of the maintenance of the oil-filled electrical equipment has been improved. Further, since the step of injecting the sample oil into the vial 1 is performed by an automatic operation, the injection time of the sample oil 2 can be reduced as compared with the conventional case, and the maintenance management of the oil-filled electric equipment is performed. Cost can be reduced. Further, as shown in FIG. 2, all the connecting points of the pipes were put together in the valve head 16, and the pipes were each provided with a check valve. As a result, the backflow of gas and oils is suppressed at all, and there is no room for any components other than the sample oil 2 to enter the vial 1 such as intrusion of air, so that the accuracy of gas analysis is further improved. Therefore, the reliability of the maintenance of the oil-filled electric equipment has been further improved.

[0013]

According to the present invention, as described above, the inside of the vial is evacuated before the carrier gas is blown off, thereby enabling the analysis of air-containing components such as O ₂ and N ₂ in gas analysis. The accuracy has been improved, and the reliability of maintenance management of oil-filled electrical equipment has become higher than before.

In this configuration, the step of evacuating the vial, the step of blowing carrier gas into the vial, and the step of injecting sample oil from the syringe into the vial are automatically operated. By doing so, it is possible to shorten the injection time of the sample oil than before,
The maintenance cost of oil-filled electrical equipment has been reduced. Also,
In such a configuration, the connection points of the pipes are collectively stored in the valve head, and the pipes are each provided with a check valve, so that there is no room for any components other than the sample oil to be mixed into the vial. The accuracy of gas analysis has been further improved, and the reliability of maintenance management of oil-filled electrical equipment has been further improved.

[Brief description of the drawings]

FIG. 1 is a perspective view showing a configuration of an apparatus for injecting a sample oil for gas analysis into a vial according to an embodiment of the present invention.

FIG. 2 is a piping system diagram of FIG.

3A and 3B are cross-sectional views illustrating the analysis principle of the headspace method, wherein FIG. 3A shows a state in which sample oil is stored in a vial, and FIG. 3B shows a state in which the vial is heated and stirred.

FIG. 4 is a partially fragmented side view showing the configuration of a conventional apparatus for injecting a sample oil for gas analysis into a vial.

[Explanation of symbols]

1: vial, 1A: clamp, 2: sample oil, 3: first
Needle, 4: Second needle, 5: Third needle, 6:
Carrier gas supply device, 10: gas filling port, 11: syringe, 16: valve head, 17: lid, 18: first check valve, 19: second check valve, 20: third check valve, 21: 4th
Check valve, 22: control box, 23: manual handle, 24: pusher, 25: air cylinder, 26:
Safety cover, 27: air hose, 27A: high pressure air, 2
7B, 28B, 29B: solenoid on-off valve, 28: vacuum pipe,
28A: air, 29: carrier gas pipe, 29A: carrier gas, 30: exhaust gas pipe, 31, 41: regulator,
32: vacuum gauge, 33: adjustment knob, 34: receiving plate, 36: vacuum exhaust device, 37: high-pressure air supply device

Claims (3)

[Claims] 1. A device for injecting a sample oil into a vial for analyzing a gas dissolved in the sample oil, wherein a first needle and a second needle are inserted into a gas filling port of the vial and a carrier is provided. A gas is blown from the first needle through the vial to the second needle, and then the sample oil collected in the syringe is injected into the vial from the first needle into a vial of the sample oil for gas analysis. Wherein the inside of the vial is evacuated before the carrier gas is blown off, wherein the sample oil for gas analysis is injected into the vial. 2. An apparatus for injecting a sample oil for gas analysis into a vial according to claim 1, wherein a step of evacuating the vial, a step of blowing carrier gas into the vial, and a step of transferring a sample from the syringe into the vial. An apparatus for injecting a sample oil for gas analysis into a vial, wherein the step of injecting oil is automatically operated. 3. The apparatus for injecting a sample oil for gas analysis into a vial according to claim 1, wherein the first and second needles inserted into the gas filling port of the vial are provided projecting downward. A valve head into which a third needle from a syringe is inserted from above, wherein the valve head communicates from the first needle to a vacuum exhaust device, and from the first needle to a carrier gas supply device. A second check valve, a third check valve communicating from the first needle to the third needle of the syringe, and a fourth check valve communicating from the second needle to the outside air. Is a device for injecting a sample oil for gas analysis into a vial, wherein the valve head is moved downward to be inserted into a gas filling port of the vial.