CN107796886A - A kind of method of propylene content in measure insulating oil - Google Patents
A kind of method of propylene content in measure insulating oil Download PDFInfo
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- CN107796886A CN107796886A CN201710883373.1A CN201710883373A CN107796886A CN 107796886 A CN107796886 A CN 107796886A CN 201710883373 A CN201710883373 A CN 201710883373A CN 107796886 A CN107796886 A CN 107796886A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- 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
- G01N30/02—Column chromatography
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Abstract
The present invention relates to a kind of method for determining propylene content in insulating oil, standard propylene gas sampling is analyzed using gas chromatograph, make the standard curve of propylene gas content and relative response of GC, insulation oil samples to be measured are taken according to hermetically sealed sampling method, the gas of dissolved in insulating oil is removed using vacuum degasser, chromatographic column is recycled to isolate propylene gas therein, using the relative response of GC of gas chromatograph detection propylene, contrast standard curve obtains the concentration of propylene gas.The content of propylene in insulating oil is determined using the method disclosed in the present, test result is accurate, can meet the requirement of Fault Diagnosis for Electrical Equipment analysis.
Description
Technical field
The present invention relates to eudiometry field, more particularly, to a kind of method for determining propylene content in insulating oil.
Background technology
Transformer, oil circuit breaker, oil-filled cable, sleeve pipe, transformer may determine that by the dissolved gas component in insulating oil
It whether there is failure or latency defect, such as hot-spot, electric discharge, insulation ag(e)ing Deng power equipment inside, it is therefore, molten in oil
It is the most important prevention of oil-filled power equipment and diagnostic test that physical examination of venting one's spleen, which is surveyed,.Determined using gas chromatography in insulating oil
Dissolved gas content is existing international method, and these gases mainly include：H2、CH4、C2H6、C2H4、C2H2、CO、CO2.Should
Before method sample introduction, balance degassing method (mechanical oscillation degassing) or vacuum degassing need to be used to carry out Oil-gas Separation, recycle gas phase
The content of each component, calculates each component content being dissolved in insulating oil on this basis in chromatograph measurement abjection gas.
With the construction and operation of the lifting of power equipment voltage class, particularly super-pressure, extra-high voltage grid, examined for equipment fault
Break to propose and more accurately more fully require, the C of dissolved in insulating oil3H6Also it is concerned therewith, but do not provide
The distribution coefficient of this component, cause effectively determine this content of the component in insulating oil using balance degassing method,
Prior art can only use full degassing method to carry out Oil-gas Separation to insulating oil, to avoid in test result using distribution
Coefficient calculates.However, either balancing degassing method or full degassing method, the method for testing of this component is not reported also at present
Road.
The content of the invention
It is an object of the present invention to overcome the above-mentioned drawbacks of the prior art and provide one kind is determined in insulating oil
The method of propylene content.
The purpose of the present invention can be achieved through the following technical solutions：
A kind of method of propylene content in measure insulating oil, it is characterised in that this method uses following steps：
(1) insulation oil samples to be measured are obtained from high voltage electric equipment according to hermetically sealed sampling method；
(2) standard propylene gas sampling is analyzed using gas chromatograph, makes propylene gas content and rung with gas-chromatography
The standard curve that should be worth；
(3) gas of dissolved in insulating oil is removed using vacuum degasser, recycles chromatographic column to isolate
Propylene gas therein, the relative response of GC of propylene is detected using gas chromatograph, and contrast standard curve obtains propylene gas
The concentration of body.
Step (2) specifically uses following steps：
(2-1) opens gas chromatograph and treats baseline stability, and observation base noise takes the baseline noise value of three times, and calculates
Method analyzes the test limit of propylene；
(2-2) is analyzed the standard propylene gas sampling of various concentrations using gas chromatograph, makes standard curve.
The standard curve for making obtained propylene gas content and relative response of GC is：
Y=6.9597x-4.7501, wherein x are propylene gas concentration, and unit μ L/L, y are relative response of GC, the mark
The range of linearity of directrix curve is 0~124 μ L/L.
Vacuum is evacuated to below 10Pa by step (3) using vacuum degasser, removes dissolved in insulating oil to be measured
Gas.The chromatographic column used for series connection Propack Q posts and 5A molecular sieve columns.The condition of gas chromatograph is as follows：
The gradient increased temperature of described Propack Q posts is 55~120 DEG C, and heating rate is 15 DEG C/min；
The gradient increased temperature of described 5A molecular sieve columns is 40~250 DEG C, and heating rate is 25 DEG C/min；
The temperature of thermal conductivity cell detector is 60 DEG C, and electric current is set to 85mA,
The temperature of hydrogen flame detector is 130 DEG C.
Compared with prior art, the present invention tests the content of propylene in insulating oil, this kind using the full Degassing Technology of vacuum
Gas shows preferable linear response, and detection is limited to 0.29 μ L/L, and the rate of recovery is between 91.1%~102.7%, measure
The relative standard deviation (n=6) of value is 3.2%, and test result is accurate, can meet wanting for Fault Diagnosis for Electrical Equipment analysis
Ask.
Brief description of the drawings
Fig. 1 is the standard curve of propylene gas content and relative response of GC；
Fig. 2 is that FID detects its baseline noise figure.
Embodiment
With reference to specific embodiment, the present invention is described in detail.Following examples will be helpful to the technology of this area
Personnel further understand the present invention, but the invention is not limited in any way.It should be pointed out that the ordinary skill to this area
For personnel, without departing from the inventive concept of the premise, various modifications and improvements can be made.These belong to the present invention
Protection domain.
The test apparatus and material used in the present embodiment
TOGA GC gas chromatographs, German ENERGY SUPPORT companies production；GC-900 gas chromatographs, Shang Haihai
Glad chromatogram Co., Ltd production；Balance degasser ZHQ701, Zhonghui Instrument Co., Ltd.；Vacuum Degassing
System vacuum degassers, German ENERGY SUPPORT companies production；Two-sided frosted syringe, the life of Wei De Man of Sweden
Production；QL-1000 hydrogen generators, Shandong Success Hydrogen Energy Co., Ltd.'s production；ZLJ-30 type Double-stage vacuum oil filters, it is safe
Zhou Hongtai power equipments Co., Ltd produces；Argon gas (Ar), Shanghai Pujiang Specialty Gases Co., Ltd.'s production, purity 99.9%；
Calibrating gas, the production of Shanghai Wei Chuan gases Co., Ltd, high and low concentration of component are listed in Tables 1 and 2.
The high standard gas content table of table 1
| Component | Content, μ L/L | Component | Content, μ L/L |
| CH4 | 748 | C2H2 | 25.3 |
| C2H6 | 295 | H2 | 1114 |
| C2H4 | 502 | CO | 1042 |
| CO2 | 1005 | C3H6 | 135 |
| C3H6 | 124 | Ar | It is remaining |
The low concentration calibrating gas content table of table 2
| Component | Content, μ L/L | Component | Content, μ L/L |
| CH4 | 7.7 | C2H2 | 0.7 |
| C2H6 | 2.9 | H2 | 9.9 |
| C2H4 | 5.2 | CO | 9.9 |
| CO2 | 10.0 | C3H6 | 5.2 |
| C3H6 | 5.2 | Ar | It is remaining |
Embodiment
A kind of method of propylene content in measure insulating oil, using following steps：
(1) after gas chromatograph starting up, treat baseline stability, observation base noise, take the baseline noise values of three times.Again
The calibrating gas sample introduction of two kinds of concentration is analyzed using gas chromatograph, utilizes the calibrating gas sample detection result of high-concentration and low-concentration
Depict C3H6Standard curve, as shown in figure 1, the standard for making obtained propylene gas content and relative response of GC is bent
Line is：Y=6.9597x-4.7501, wherein x are propylene gas concentration, and unit μ L/L, y are relative response of GC, from figure
As can be seen that C3H6Coefficient correlation be respectively 0.9999, the range of linearity is 0~124 μ L/L, and it is preferable to show that the component all has
Linear response；
(2) insulation oil samples to be measured are taken according to hermetically sealed sampling method, using vacuum degasser to molten in insulating oil
The gas of solution is removed, and recycles chromatographic column to isolate propylene gas therein, and the gas of propylene is detected using gas chromatograph
Phase chromatogram response, contrast standard curve obtain the concentration of propylene gas.
Vacuum is evacuated to below 10Pa using vacuum degasser, the gas of dissolved in insulating oil to be measured is removed, adopts
Chromatographic column is the Propack Q posts and 5A molecular sieve columns of series connection, and the gradient increased temperature of Propack Q posts is 55~120 DEG C, is risen
Warm speed is 15 DEG C/min, and the gradient increased temperature of 5A molecular sieve columns is 40~250 DEG C, and heating rate is 25 DEG C/min；Conductance cell is examined
The temperature for surveying device (TCD) is 60 DEG C, 85mA, and the temperature of hydrogen flame detector (FID) is 130 DEG C.
The vacuum of the system of degassing is evacuated to below 10Pa, insulating oil profit to be measured by Gas analysis first with vavuum pump
Degassing room is discharged into pressure differential, is deaerated full method using vacuum, the gas of dissolved in insulating oil is escaped, and by the gas of escape
Collection chamber is stored in, carrier gas with pressure will deviate from gas ejection.By the gas after discharge from injection port sample introduction, pass through determining for 500 μ L
Ring control sample size is measured, first, chromatographic column 1 (Propack Q posts) and chromatographic column 2 (5A molecular sieve columns) series connection are by under test gas
H2、O2、N2Separation, is then turned off series valve, using only post 1 by CO2、C2H4、C2H6、C2H2Separation, again beats series valve
Open, Propack Q posts and 5A molecular sieve columns are combined CH4、CO、C3H6Separation.
The test limit of gas chromatograph can be calculated using 3 times of baseline noise, as shown in Equation 1
D=3N*Q/I (1)
In formula：D-detection limit, N-noise, Q-sample size, I-signal response
FID detects its baseline noise as shown in Fig. 2 it can be seen that baseline noise approaches after chromatograph is stable
0.5 μ V, substituting into formula (1) using the concentration and peak height of calibrating gas can obtain, and gas chromatograph is for C in gas3H6Test limit
Respectively 0.33 μ L/L.
The test of dissolved gas each component, knot are carried out to the insulating oil after the processing of its vacuum oil-filter using gas chromatograph
Fruit is listed in table 3, as can be known from the results of Table 3, although also containing some other components in blank oil after processing, has not contained
The C to be detected3H6.Using this method, the insulating oil for being separately added into 2ml, 3ml, 4ml, 6ml high standard gas is carried out
C3H6Content measuring, test result are listed in table 4, as can be seen from Table 4, C3H6The rate of recovery be 91.9%~107.9%.
The dissolved gas content of insulating oil after the processing of the vacuum oil-filter of table 3
| Component | Content, μ L/L | Component | Content, μ L/L |
| CO2 | 5.6 | Hydrogen | 0 |
| Ethene | 0.41 | C3H6 | 0 |
| Ethane | 0.24 | C3H8 | 0 |
| Methane | 0.95 | Acetylene | 0 |
| Carbon monoxide | 1.6 |
The recovery test result of table 4
6 insulation oil samples that No. 4 main transformers in station are run to Guo Wang companies carry out C3H6Assay, test result is arranged
In table 5.From the results shown in Table 5：C3H66 measurement result standard deviations be respectively 6.8%.
The measurement result of certain No. 4 main change insulated oil samples in station of table 5
| Sample number into spectrum | C3H6, μ L/L |
| 1 | 231 |
| 2 | 219 |
| 3 | 222 |
| 4 | 238 |
| 5 | 224 |
| 6 | 233 |
| RSD, % | 3.2 |
C in insulating oil is tested using the full Degassing Technology of vacuum3H6Content, show preferable linear response, detect
0.29 μ L/L are limited to, the rate of recovery is repeated between 91.9%~107.9% to the oil samples that insulated in 6 operational outfits
Property test, the relative standard deviation (n=6) of measured value is 3.2%.
The specific embodiment of the present invention is described above.It is to be appreciated that the invention is not limited in above-mentioned
Particular implementation, those skilled in the art can make various deformations or amendments within the scope of the claims, this not shadow
Ring the substantive content of the present invention.
Claims (6)
- A kind of 1. method for determining propylene content in insulating oil, it is characterised in that this method uses following steps：(1) insulation oil samples to be measured are obtained from high voltage electric equipment according to hermetically sealed sampling method；(2) standard propylene gas sampling is analyzed using gas chromatograph, makes propylene gas content and relative response of GC Standard curve；(3) gas of dissolved in insulating oil is removed using vacuum degasser, recycles chromatographic column to isolate wherein Propylene gas, the relative response of GC of propylene is detected using gas chromatograph, contrast standard curve obtains propylene gas Concentration.
- 2. a kind of method for determining propylene content in insulating oil according to claim 1, it is characterised in that step (2) has Body uses following steps：(2-1) opens gas chromatograph and treats baseline stability, observation base noise, takes the baseline noise value of three times, and computational methods Analyze the test limit of propylene；(2-2) is analyzed the standard propylene gas sampling of various concentrations using gas chromatograph, makes standard curve.
- 3. a kind of method for determining propylene content in insulating oil according to claim 1 or 2, it is characterised in that be made to To propylene gas content and the standard curve of relative response of GC be：Y=6.9597x-4.7501, wherein x are propylene gas concentration, and unit μ L/L, y are relative response of GC, and the standard is bent The range of linearity of line is 0~124 μ L/L.
- A kind of 4. method for determining propylene content in insulating oil according to claim 1, it is characterised in that step (3) profit Vacuum is evacuated to below 10Pa with vacuum degasser, removes the gas of dissolved in insulating oil to be measured.
- 5. a kind of method for determining propylene content in insulating oil according to claim 1, it is characterised in that in step (3) The chromatographic column used for series connection Propack Q posts and 5A molecular sieve columns.
- 6. a kind of method for determining propylene content in insulating oil according to claim 5, it is characterised in that in step (3) The condition of the gas chromatograph of use is as follows：The gradient increased temperature of described Propack Q posts is 55~120 DEG C, and heating rate is 15 DEG C/min；The gradient increased temperature of described 5A molecular sieve columns is 40~250 DEG C, and heating rate is 25 DEG C/min；The temperature of thermal conductivity cell detector is 60 DEG C, and electric current is set to 85mA,The temperature of hydrogen flame detector is 130 DEG C.
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| CN201710883373.1A CN107796886A (en) | 2017-09-26 | 2017-09-26 | A kind of method of propylene content in measure insulating oil |
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| CN201710883373.1A CN107796886A (en) | 2017-09-26 | 2017-09-26 | A kind of method of propylene content in measure insulating oil |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112630326A (en) * | 2020-12-02 | 2021-04-09 | 南通醋酸纤维有限公司 | Method for measuring content of dissolved gas organic matters in liquid |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE10252652A1 (en) * | 2002-11-11 | 2004-05-19 | Ech Elektrochemie Halle Gmbh | Apparatus analyzing gas content of transformer-, lubricating-, engine and hydraulic oils or aqueous solutions, comprises mercury-free vacuum pump for degasification |
| CN104076102A (en) * | 2014-07-01 | 2014-10-01 | 长沙业嘉电子科技有限公司 | Analyzer for gas dissolved in mobile type insulating oil and detection method of gas dissolved in mobile type insulating oil |
| CN106370746A (en) * | 2016-08-26 | 2017-02-01 | 湖南大学 | Gas-dissolved-in-vegetable-insulating-oil analyzer with oil-gas separation function and detecting method |
-
2017
- 2017-09-26 CN CN201710883373.1A patent/CN107796886A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE10252652A1 (en) * | 2002-11-11 | 2004-05-19 | Ech Elektrochemie Halle Gmbh | Apparatus analyzing gas content of transformer-, lubricating-, engine and hydraulic oils or aqueous solutions, comprises mercury-free vacuum pump for degasification |
| CN104076102A (en) * | 2014-07-01 | 2014-10-01 | 长沙业嘉电子科技有限公司 | Analyzer for gas dissolved in mobile type insulating oil and detection method of gas dissolved in mobile type insulating oil |
| CN106370746A (en) * | 2016-08-26 | 2017-02-01 | 湖南大学 | Gas-dissolved-in-vegetable-insulating-oil analyzer with oil-gas separation function and detecting method |
Non-Patent Citations (4)
| Title |
|---|
| 刘尧 等: "《无机及分析化学》", 31 December 2003 * |
| 孟玉婵 等: "《中华人民共和国国家标准GB/T 17623-2017 绝缘油中的溶解气体组分含量的气相色谱测定法》", 12 May 2017 * |
| 董艳波: "气相色谱法测定绝缘油中溶解气体组分总含气量方法与应用", 《民营科技》 * |
| 黄云光 等: "单柱流程油气色谱分析技术", 《广西电力技术》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112630326A (en) * | 2020-12-02 | 2021-04-09 | 南通醋酸纤维有限公司 | Method for measuring content of dissolved gas organic matters in liquid |
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