CN112305130A - Preposed automatic degassing sample introduction device and method for transformer oil chromatography - Google Patents
Preposed automatic degassing sample introduction device and method for transformer oil chromatography Download PDFInfo
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- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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Abstract
The invention relates to a preposed automatic degassing and sampling device and a method for transformer oil chromatography. Belongs to the technical field of transformer oil chromatographic detection. The quantitative oil cylinder is connected with an inlet of the degassing chamber, the nitrogen gas inlet pipe is connected with an inlet of the degassing chamber, an air inlet pipeline of the vacuum pump is connected with an outlet of the degassing chamber, an air outlet pipeline of the vacuum pump is connected with one end of a communication circulating pipe, the other end of the communication circulating pipe is connected with an inlet of the degassing chamber, the outlet is located at the top of the degassing chamber, the inlet is located at the bottom of the degassing chamber, and the inlet is located at the bottom of the degassing chamber. The method combining vacuum degassing and dynamic headspace degassing solves the problems that the degassing rate of the existing vacuum degassing device is unstable and cannot be well controlled. The problem of manual advance kind calibration error is solved.
Description
Technical Field
The invention belongs to the technical field of transformer oil chromatographic detection, and particularly relates to a front automatic degassing and sampling device and method for transformer oil chromatography.
Background
The information in this background section is only for enhancement of understanding of the general background of the invention and is not necessarily to be construed as an admission or any form of suggestion that this information forms the prior art that is already known to a person of ordinary skill in the art.
The analysis of the dissolved gas in the transformer oil is to perform gas chromatography detection analysis on the characteristic gas dissolved in the transformer oil to judge the internal operation condition of the oil-filled electrical equipment. The chromatographic analysis of the transformer oil mainly comprises two steps: degassing and sample analysis, wherein degassing refers to the removal of characteristic gases dissolved in the transformer oil, which is a prerequisite for sample analysis. The most widely used degassing method is a mechanical oscillation method, but the mechanical oscillation method has many manual operation steps, and a single sample has long detection time, which easily causes detection errors.
At present, partial units select a vacuum degassing device to replace a mechanical oscillation method, compared with the mechanical oscillation method, the vacuum method has the advantages of less manual operation, short degassing time and lower minimum detection concentration, but the problems of unstable degassing rate, poor repeatability and the like still exist in the current vacuum method, and particularly the accuracy of transformer oil sample detection is seriously influenced by the vacuum degassing device with longer application time. Meanwhile, when the vacuum degassing method is applied currently, the gas chromatograph is calibrated by adopting a method of manually feeding standard gas, the transformer oil sample is automatically fed by an automatic degassing and sampling device, and the difference of the sample volumes of the transformer oil sample and the automatic degassing and sampling device can cause the final detection result to have errors.
Disclosure of Invention
Aiming at the problems in the prior art, the invention aims to provide a preposed automatic degassing sampling device and a method for transformer oil chromatography.
In order to solve the technical problems, the technical scheme of the invention is as follows:
according to the first aspect, the preposed automatic degassing and sampling device for the transformer oil chromatography comprises a degassing chamber, a quantitative oil cylinder, a nitrogen gas inlet pipe and a vacuum pump, wherein an inlet of the degassing chamber is connected with the quantitative oil cylinder, an atomizing nozzle is arranged at an inlet in the degassing chamber, the nitrogen gas inlet pipe is connected with an inlet of the degassing chamber, an air inlet pipeline of the vacuum pump is connected with an outlet of the degassing chamber, an air outlet pipeline of the vacuum pump is connected with one end of a communicating circulating pipe, the other end of the communicating circulating pipe is connected with an inlet of the degassing chamber, the outlet is located at the top of the degassing chamber, the inlet is located at the bottom of the degassing chamber.
The method combining vacuum degassing and dynamic headspace degassing solves the problems that the degassing rate of the existing vacuum degassing device is unstable and cannot be well controlled. The problem of manual advance kind calibration error is solved.
In a second aspect, a degassing and sample injection method of a preposed automatic degassing and sample injection device for transformer oil chromatography comprises the following specific steps:
injecting a quantitative standard gas into a gas chromatograph for external standard calibration;
flushing the degassing chamber and the quantitative pipe with nitrogen, evacuating with a vacuum pump, introducing the oil sample into the degassing chamber, the quantitative oil cylinder and the pipeline, and evacuating the oil sample;
opening a vacuum pump to vacuumize to reach the required pressure;
the quantitative oil enters a quantitative oil cylinder through an oil inlet pipe for quantification;
the quantitative oil cylinder enables an oil sample to enter a degassing chamber, nitrogen is filled in the degassing chamber to supplement air, a vacuum pump is used for leading out gas from the upper part of the degassing chamber and injecting the gas from the lower part of the degassing chamber to form a circulation loop, dynamic headspace degassing and vacuum degassing under a vacuum environment are combined, and the degassing step is repeated for three times to achieve a stable degassing rate;
and after degassing, collecting the gas degassed from the degassing chamber into a first quantitative tube, connecting a gas chromatograph by using a first six-way valve and a second six-way valve, and introducing a gas sample in the first quantitative tube into the gas chromatograph.
One or more technical schemes of the invention have the following beneficial effects:
the automatic degassing and sampling device is characterized in that a certain amount of nitrogen is supplemented to realize dynamic headspace degassing on the premise of ensuring a vacuum environment, the difficult problem that degassing rate is unstable and difficult to control in a common vacuum degassing device is solved by utilizing a method of combining vacuum degassing and dynamic headspace degassing, meanwhile, a standard mixed gas for calibrating a gas chromatograph is accessed into the device, the consistency of sample injection volumes of a gas sample obtained after degassing of a standard gas and an oil sample is ensured, the automatic calibration of the gas chromatograph is realized, the problem that detection errors are possibly caused by manual sampling calibration is solved, the accuracy and reliability of analysis results of dissolved gas in transformer oil are ensured, and the operation state of electrical equipment is favorably and truly judged.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this specification, are included to provide a further understanding of the invention, and are incorporated in and constitute a part of this specification, illustrate exemplary embodiments of the invention and together with the description serve to explain the invention and not to limit the invention.
FIG. 1 is a diagram of a front automatic degassing sampling device for transformer oil chromatography;
wherein, 1: a nitrogen inlet pipe; 2: a fourth solenoid valve; 3: a seventh electromagnetic valve; 4: a first pressure sensor; 5: a degassing chamber; 6: a first solenoid valve; 7: a sixth electromagnetic valve; 8: the circulating valve is communicated; 9: a degassing air inlet valve; 10: a second pressure sensor; 11: a first dosing tube; 12: a first six-way valve; 13: a tenth solenoid valve; 14: a quantitative oil cylinder; 15: a second solenoid valve; 16: a fifth solenoid valve; 17: an oil inlet pipe; 18: a second six-way valve; 19: a standard gas sample inlet pipe; 20: a standard gas inlet valve; 21: a second dosing tube; 22: a carrier gas outlet line; 23: a carrier gas inlet line; 24: an oil discharge pipe; 25: a vacuum pump; 26: an eighth solenoid valve; 27: a ninth electromagnetic valve; 28: emptying the pipe; 29: and a third solenoid valve.
Detailed Description
It is to be understood that the following detailed description is exemplary and is intended to provide further explanation of the invention as claimed. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this disclosure belongs.
It is noted that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of example embodiments according to the present disclosure. As used herein, the singular forms "a", "an" and "the" are intended to include the plural forms as well, and it should be understood that when the terms "comprises" and/or "comprising" are used in this specification, they specify the presence of stated features, steps, operations, devices, components, and/or combinations thereof, unless the context clearly indicates otherwise.
A front-end automatic degassing and sampling device for transformer oil chromatography comprises a degassing chamber, a quantitative oil cylinder, a nitrogen gas inlet pipe and a vacuum pump, wherein an inlet of the degassing chamber is connected with the quantitative oil cylinder, an atomizing nozzle is arranged at an inlet in the degassing chamber, the nitrogen gas inlet pipe is connected with an inlet of the degassing chamber, an air inlet pipeline of the vacuum pump is connected with an outlet of the degassing chamber, an air outlet pipeline of the vacuum pump is connected with one end of a communicating circulating pipe, the other end of the communicating circulating pipe is connected with an inlet of the degassing chamber, the outlet is positioned at the top of the degassing chamber, the inlet is positioned at the bottom of the degassing chamber, and the.
The method combining vacuum degassing and dynamic headspace degassing solves the problems that the degassing rate of the existing vacuum degassing device is unstable and cannot be well controlled. The problem of manual advance kind calibration error is solved.
As a further technical scheme, a first electromagnetic valve is arranged at a position, close to an inlet of the degassing chamber, on a pipeline for connecting the degassing chamber with the quantitative oil cylinder.
As a further technical scheme, a second electromagnetic valve is arranged at a position close to the quantitative oil cylinder on a pipeline connecting the degassing chamber and the quantitative oil cylinder.
As a further technical scheme, a communication circulating valve is arranged on the communication circulating pipe.
As a further technical scheme, a nitrogen gas inlet pipe is connected with an outlet of the degassing chamber, and a third electromagnetic valve and a fourth electromagnetic valve are respectively arranged on pipelines which are connected with an inlet and an outlet of the nitrogen gas inlet pipe and the degassing chamber.
As a further technical scheme, the quantitative oil cylinder further comprises an oil inlet pipe, and the oil inlet pipe is connected with the quantitative oil cylinder. And the oil inlet pipe is provided with a fifth electromagnetic valve.
The degassing device also comprises an oil discharge pipe, and the oil discharge pipe is connected with the bottom of the degassing chamber. And a sixth electromagnetic valve is arranged on the oil discharge pipe.
As a further technical scheme, a seventh electromagnetic valve and an eighth electromagnetic valve are arranged on a pipeline for connecting the vacuum pump and the degassing chamber, the seventh electromagnetic valve is arranged between a connector for connecting the degassing chamber and the nitrogen inlet pipe, and the eighth electromagnetic valve is arranged between the vacuum pump and the nitrogen inlet pipe.
As a further technical scheme, the device also comprises an emptying pipe, wherein one end of the emptying pipe is connected with the air outlet pipeline, and the emptying pipe is positioned at the upstream of the communicated circulating pipe. And a ninth electromagnetic valve is arranged on the emptying pipe.
As a further technical scheme, the device also comprises a first six-way valve and a first quantitative pipe, wherein the first quantitative pipe is connected with the first six-way valve, the vacuum pump is connected with the quantitative oil cylinder through an air outlet pipeline, the first six-way valve is arranged on the air outlet pipeline, and the first six-way valve is positioned at the downstream of the circulating communicating pipe.
As a further technical scheme, the device also comprises a second six-way valve and a second quantitative pipe, wherein the second quantitative pipe is connected with the second six-way valve, the second six-way valve is connected with the first six-way valve, and the first six-way valve and the second six-way valve are respectively connected with a carrier gas inlet pipeline and a carrier gas outlet pipeline.
As a further technical scheme, the gas sampling device further comprises a standard gas sampling pipe, and the standard gas sampling pipe is connected with the second six-way valve. And a standard gas inlet valve is arranged on the standard gas sampling pipe.
As a further technical solution, the degassing device further comprises a first pressure sensor, and the first pressure sensor is arranged at the position of a top outlet of the degassing chamber.
As a further technical scheme, the six-way valve further comprises a second pressure sensor, and the second pressure sensor is arranged at the degassing inlet position of the second six-way valve.
In a second aspect, a degassing and sample injection method of a preposed automatic degassing and sample injection device for transformer oil chromatography comprises the following specific steps:
injecting a quantitative standard gas into a gas chromatograph for external standard calibration;
flushing the degassing chamber and the quantitative pipe with nitrogen, evacuating with a vacuum pump, introducing the oil sample into the degassing chamber, the quantitative oil cylinder and the pipeline, and evacuating the oil sample;
opening a vacuum pump to vacuumize to reach the required pressure;
the quantitative oil enters a quantitative oil cylinder through an oil inlet pipe for quantification;
the quantitative oil cylinder enables an oil sample to enter a degassing chamber, nitrogen is filled in the degassing chamber to supplement air, a vacuum pump is used for leading out gas from the upper part of the degassing chamber and injecting the gas from the lower part of the degassing chamber to form a circulation loop, dynamic headspace degassing and vacuum degassing under a vacuum environment are combined, and the degassing step is repeated for three times to achieve a stable degassing rate;
and after degassing, collecting the gas degassed from the degassing chamber into a first quantitative tube, connecting a gas chromatograph by using a first six-way valve and a second six-way valve, and introducing a gas sample in the first quantitative tube into the gas chromatograph.
And after the gas sample is injected into the gas chromatograph, the degassing chamber and the quantitative oil cylinder are subjected to oil discharge and nitrogen cleaning.
As shown in fig. 1, the automatic degassing and sampling apparatus includes a degassing chamber 5, a quantitative oil cylinder 14, a nitrogen gas inlet pipe 1, and a vacuum pump 25, wherein an inlet of the degassing chamber 5 is connected to the quantitative oil cylinder 14, the nitrogen gas inlet pipe 1 is connected to an inlet and an outlet of the degassing chamber 5, one end of an inlet of the vacuum pump 25 is connected to an outlet of the degassing chamber 5, the outlet is located at the top of the degassing chamber 5, the inlet is located at the bottom of the degassing chamber 5, and the inlet is located at the bottom of the degassing chamber.
The oil sample in the quantitative oil cylinder 14 enters the degassing chamber 5, the bottom of the degassing chamber 5 is provided with a sample inlet and an inlet, and the top is provided with an outlet. Thus, after entering degassing chamber 5, the oil sample is in the bottom and in the upper gas phase. During degassing, gas escapes from the oil sample into the gas phase.
The atomizing nozzle is used for increasing the contact area when the transformer oil sample enters the degassing chamber, and the process that the oil sample enters the degassing chamber through the atomizing nozzle in a vacuum environment is equivalent to primary vacuum degassing.
The nitrogen gas inlet pipe 1 is connected with an inlet and an outlet of the degassing chamber 5, and the nitrogen gas inlet pipe 1 fills nitrogen gas into the degassing chamber through the inlet of the degassing chamber 5 to supplement the gas into the degassing chamber 5 so as to maintain the pressure in the degassing chamber 5 within a certain pressure range.
After the degassing chamber has been charged, the nitrogen inlet 1 is then closed. A circulation pipeline is formed among the degassing chamber 5, the vacuum pump 25 and the communication circulation pipe. The vacuum pump 25 pumps out the gas in the degassing chamber 5, returns to the degassing chamber through a communication circulation pipe, enters the degassing chamber 5 from the bottom of the degassing chamber 5, and then discharges the gas from the top of the degassing chamber 5. And then recycled. During the circulation process, the combination of dynamic headspace degassing and vacuum degassing is realized to carry out oil sample degassing so as to achieve stable degassing rate. And a communication circulating valve 8 is arranged on the communication circulating pipe.
The gas from the degassing chamber is discharged and re-enters the degassing chamber. The degassing chamber is always maintained in a certain pressure range to keep the relative vacuum environment of the degassing chamber, realize the vacuum degassing of the oil sample and keep the vacuum degassing. After a certain amount of nitrogen is supplemented, the removed gas is circulated by using a vacuum pump and enters from the bottom of a degassing chamber to achieve the effect of purging the transformer oil sample, namely the principle of dynamic headspace degassing, the characteristic gas components in the oil sample are continuously replaced by continuously purging the transformer oil sample by the gas, so that the effect of separating each gas component from the oil is achieved, and because the degassing chamber always maintains a relatively vacuum environment, the degassing process is equivalent to the combination of vacuum degassing and dynamic headspace degassing, and two degassing modes are simultaneously carried out to ensure that a degassing device can achieve stable degassing efficiency.
A first electromagnetic valve 6 is arranged on a pipeline of the degassing chamber 5 connected with the quantitative oil cylinder 14 and is close to the inlet. The sample introduction and gas admission to the degassing chamber 5 are controlled. A second electromagnetic valve 15 is arranged on the pipeline of the degassing chamber 5 connected with the quantitative oil cylinder 14 and close to the quantitative oil cylinder. And controlling the sample output of the quantitative oil cylinder.
And a nitrogen inlet pipe is connected with an outlet of the degassing chamber, and a pipeline connecting the nitrogen inlet pipe with the inlet and the outlet of the degassing chamber is respectively provided with a third electromagnetic valve 29 and a fourth electromagnetic valve 2. The solenoid valve on the nitrogen inlet pipe 1 controls the delivery of gas.
The quantitative oil cylinder also comprises an oil inlet pipe 17, and the oil inlet pipe 17 is connected with the quantitative oil cylinder 14. The oil inlet pipe is provided with a fifth electromagnetic valve 16. The oil inlet pipe 17 conveys oil samples to the quantitative oil cylinder.
An oil drain pipe 24 is also included, the oil drain pipe 24 being connected to the bottom of the degassing chamber 5. The sixth electromagnetic valve 7 is arranged on the oil discharge pipe 24. The oil drain pipe 24 is used for discharging the oil sample after degassing the oil sample.
A seventh electromagnetic valve 3 and an eighth electromagnetic valve 26 are arranged on the pipeline of the vacuum pump 25 connected with the degassing chamber 5, the seventh electromagnetic valve 3 is arranged between the interface of the degassing chamber 5 and the nitrogen inlet pipe 1, and the eighth electromagnetic valve 26 is arranged between the vacuum pump 25 and the nitrogen inlet pipe 1.
And the air exhaust pipe 28 is also included, one end of the air exhaust pipe 28 is connected with the air outlet pipeline, and the air exhaust pipe 28 is positioned at the upstream of the communication circulation pipe. The evacuation pipe is provided with a ninth solenoid valve 27.
The quantitative oil pump further comprises a first six-way valve 12 and a first quantitative pipe 11, wherein the first quantitative pipe 11 is connected with the first six-way valve 12, a vacuum pump 25 is connected with the quantitative oil cylinder 14 through an air outlet pipeline, the first six-way valve 12 is arranged on the air outlet pipeline, and the first six-way valve 12 is located on the downstream of the circulating communicating pipe. And a degassing air inlet valve 9 is also arranged, and the degassing air inlet valve 9 is arranged at the downstream of a connecting port of the circulating communicating pipe and the air outlet pipeline. Downstream is in the direction of the outlet of the vacuum pump 25. A tenth electromagnetic valve 13 is arranged on a pipeline connecting the first six-way valve 12 and the degassing chamber 5. The gas pumped by the vacuum pump 25 is conveyed to the first dosing pipe 11.
The device also comprises a second six-way valve 18 and a second quantitative pipe 21, wherein the second quantitative pipe 21 is connected with the second six-way valve 18, the second six-way valve 18 is connected with the first six-way valve 12, and the first six-way valve 12 and the second six-way valve 18 are respectively connected with a carrier gas inlet pipeline 23 and a carrier gas outlet pipeline 22. And the gas sampling device also comprises a standard gas sampling pipe 19, and the standard gas sampling pipe 19 is connected with the second six-way valve 18. The standard gas inlet pipe is provided with a standard gas inlet valve 20.
The first six-way valve 12 delivers the gas sample to the gas chromatograph and the second six-way valve delivers the standard gas to the gas chromatograph.
A first pressure sensor 4 is also included, the first pressure sensor 4 being arranged at the top outlet position of the degassing chamber. The first pressure sensor 4 is used to detect the gas pressure at the degassing chamber outlet.
A second pressure sensor 10 is also included, the second pressure sensor 10 being arranged at the degassing inlet of the second six-way valve 18. The second pressure sensor 10 is used to detect the air pressure at the inlet of the second six-way valve 18.
The method for degassing by using the automatic degassing and sampling device comprises the following specific steps:
1) calibration of a gas chromatograph: the standard gas sample introduction pipe 19 is connected with the standard mixed gas, the standard gas inlet valve 20 is opened, the standard gas is quantified through the second quantifying pipe 21, and through the switching of the second six-way valve 18 and the first six-way valve 12, under the condition that the gas chromatograph is prepared, the carrier gas passes through the second quantifying pipe 21, and the quantified standard gas is injected into the gas chromatograph to be calibrated by an external standard method.
2) Cleaning of the degassing device: the oil inlet pipe 17 is connected to the oil sample, and the electromagnetic valves 2, 3, 6, 15, 13, 9, 27 are first opened, the degassing chamber 5, the first metering pipe 11, and the like are gas-purged with nitrogen gas, and all the electromagnetic valves are closed. The vacuum pumps are then evacuated by opening the solenoid valves 26, 3, 6, 15, evacuating the nitrogen and closing all the solenoid valves. And finally, opening the electromagnetic valves 16, 15 and 6, enabling the oil inlet pipe 17 to enter the small amount of oil sample cleaning and degassing chamber 5, the quantitative oil cylinder 14 and the pipeline, closing all the electromagnetic valves, and emptying the oil sample after cleaning.
3) Vacuumizing: the vacuum pump 25 is turned on, the electromagnetic valves 3 and 26 are opened, the degassing chamber 5 is evacuated, and the operation is repeated three times until the pressure in the degassing chamber 5 is stabilized to a desired pressure.
4) Oil inlet: the electromagnetic valve 15 is opened, and the oil sample enters the quantitative oil cylinder 14 for quantitative determination through the oil inlet pipe 17.
5) Degassing: opening the electromagnetic valves 15 and 6, enabling the oil sample to enter the degassing chamber 5 from the quantitative oil cylinder 14 through the atomizing nozzle, wherein the entering process of the oil sample is equivalent to primary degassing, closing the electromagnetic valves 15 and 6, then opening the electromagnetic valves 26 and 6, filling a small amount of nitrogen for gas supplementation, ensuring the pressure of the degassing chamber within a certain range through the first pressure sensor 4, maintaining the vacuum environment, closing the electromagnetic valves 26 and 6 after the gas supplementation is finished, opening the electromagnetic valves 3, 26, 8 and 6, leading out the gas from the upper part of the degassing chamber 5 by using the vacuum pump 25, injecting the gas from the lower part of the degassing chamber 5, achieving a circulation loop, and realizing the combination of dynamic headspace degassing and vacuum degassing in the vacuum environment. The degassing step was repeated three times to achieve a stable degassing rate.
6) Gas collection: after degassing is completed, degassing inlet valve 9 is opened, the gas emerging from degassing chamber 5 is collected in first dosing pipe 11 and second pressure sensor 10 is observed.
7) Sample injection analysis: and (3) switching on the gas chromatograph by using the first six-way valve 12 and the second six-way valve 18, and injecting the gas sample in the first quantitative tube 11 into the gas chromatograph by using the carrier gas for quantitative analysis.
8) Oil discharge and cleaning: after the oil sample is degassed and the sample analysis of the gas sample is completed, the degassing chamber 5 and the quantitative oil cylinder 14 are subjected to oil discharge and nitrogen purging to prepare for the next sample detection.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. The utility model provides a transformer oil chromatogram is with leading automatic degassing sampling device which characterized in that: the device comprises a degassing chamber, a quantitative oil cylinder, a nitrogen inlet pipe and a vacuum pump, wherein an inlet of the degassing chamber is connected with the quantitative oil cylinder, an atomizing nozzle is arranged at the inlet of the degassing chamber, the nitrogen inlet pipe is connected with an inlet of the degassing chamber, an inlet pipeline of the vacuum pump is connected with an outlet of the degassing chamber, an outlet pipeline of the vacuum pump is connected with one end of a communicating circulating pipe, the other end of the communicating circulating pipe is connected with an inlet of the degassing chamber, the outlet is positioned at the top of the degassing chamber, the inlet is positioned at the bottom of the degassing chamber, and the inlet is.
2. The transformer oil chromatogram front automatic degassing sampling device of claim 1, which is characterized in that: a first electromagnetic valve is arranged at a position, close to an inlet of the degassing chamber, on a pipeline connecting the degassing chamber and the quantitative oil cylinder;
or a second electromagnetic valve is arranged on a pipeline connecting the degassing chamber and the quantitative oil cylinder and close to the quantitative oil cylinder;
or a communication circulating valve is arranged on the communication circulating pipe.
3. The transformer oil chromatogram front automatic degassing sampling device of claim 1, which is characterized in that: the nitrogen inlet pipe is connected with an outlet of the degassing chamber, and a third electromagnetic valve and a fourth electromagnetic valve are respectively arranged on pipelines connected with an inlet and an outlet of the degassing chamber.
4. The transformer oil chromatogram front automatic degassing sampling device of claim 1, which is characterized in that: the quantitative oil cylinder is characterized by further comprising an oil inlet pipe, and the oil inlet pipe is connected with the quantitative oil cylinder. And the oil inlet pipe is provided with a fifth electromagnetic valve.
5. The transformer oil chromatogram front automatic degassing sampling device of claim 1, which is characterized in that: the degassing device also comprises an oil discharge pipe, and the oil discharge pipe is connected with the bottom of the degassing chamber.
6. The transformer oil chromatogram front automatic degassing sampling device of claim 1, which is characterized in that: a seventh electromagnetic valve and an eighth electromagnetic valve are arranged on a pipeline for connecting the vacuum pump with the degassing chamber, the seventh electromagnetic valve is arranged between the degassing chamber and a connector for connecting the nitrogen inlet pipe, and the eighth electromagnetic valve is arranged between the vacuum pump and the nitrogen inlet pipe;
or the air conditioner also comprises an emptying pipe, one end of the emptying pipe is connected with the air outlet pipeline, and the emptying pipe is positioned at the upstream of the communicating and circulating pipe.
7. The transformer oil chromatogram front automatic degassing sampling device of claim 1, which is characterized in that: the device also comprises a first six-way valve and a first quantitative pipe, wherein the first quantitative pipe is connected with the first six-way valve, the vacuum pump is connected with the quantitative oil cylinder through an air outlet pipeline, the first six-way valve is arranged on the air outlet pipeline, and the first six-way valve is positioned at the downstream of the circulating communicating pipe.
8. The transformer oil chromatogram front automatic degassing sampling device of claim 7, which is characterized in that: the device also comprises a second six-way valve and a second quantitative pipe, wherein the second quantitative pipe is connected with the second six-way valve, the second six-way valve is connected with the first six-way valve, and the first six-way valve and the second six-way valve are respectively connected with the carrier gas inlet pipeline and the carrier gas outlet pipeline.
9. The transformer oil chromatogram front automatic degassing sampling device of claim 1, which is characterized in that: the standard gas sampling pipe is connected with the second six-way valve;
or, further comprising a first pressure sensor disposed at a top outlet location of the degassing chamber;
or, the device also comprises a second pressure sensor which is arranged at the degassing inlet position of the second six-way valve.
10. The degassing and sample injection method by using the preposed automatic degassing and sample injection device for the transformer oil chromatography as claimed in any one of claims 1 to 9, is characterized in that: the method comprises the following specific steps:
injecting a quantitative standard gas into a gas chromatograph for external standard calibration;
flushing the degassing chamber and the quantitative pipe with nitrogen, evacuating with a vacuum pump, introducing the oil sample into the degassing chamber, the quantitative oil cylinder and the pipeline, and evacuating the oil sample;
opening a vacuum pump to vacuumize to reach the required pressure;
the quantitative oil enters a quantitative oil cylinder through an oil inlet pipe for quantification;
the quantitative oil cylinder enables an oil sample to enter a degassing chamber, nitrogen is filled in the degassing chamber to supplement air, a vacuum pump is used for leading out gas from the upper part of the degassing chamber and injecting the gas from the lower part of the degassing chamber to form a circulation loop, dynamic headspace degassing and vacuum degassing under a vacuum environment are combined, and the degassing step is repeated for three times to achieve a stable degassing rate;
and after degassing, collecting the gas degassed from the degassing chamber into a first quantitative tube, connecting a gas chromatograph by using a first six-way valve and a second six-way valve, and introducing a gas sample in the first quantitative tube into the gas chromatograph.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011328921.2A CN112305130A (en) | 2020-11-24 | 2020-11-24 | Preposed automatic degassing sample introduction device and method for transformer oil chromatography |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011328921.2A CN112305130A (en) | 2020-11-24 | 2020-11-24 | Preposed automatic degassing sample introduction device and method for transformer oil chromatography |
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| CN112305130A true CN112305130A (en) | 2021-02-02 |
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| CN113334607A (en) * | 2021-06-09 | 2021-09-03 | 海德里希(厦门)真空机械制造有限公司 | Multi-component mixing device for wind power blade production and control method thereof |
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