CN109799293A - The detection method and its application of concentration of alcohol in a kind of transformer insulation oil - Google Patents
The detection method and its application of concentration of alcohol in a kind of transformer insulation oil Download PDFInfo
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Abstract
The invention discloses the detection method and its application of concentration of alcohol in a kind of transformer insulation oil, detection method includes: that the obtained reference substance solution of DMSO constant volume is added in ethyl alcohol, and transformer insulation oil is extracted by DMSO and test solution is made；Reference substance solution and test solution are detected respectively using gas-chromatography and mass spectrometry, obtain concentration of alcohol in transformer insulation oil.And disclose application of the detection method in terms of determining power transformer Aging of Oil-paper Insulation in Oil.The present invention provides a kind of new means for the assessment of insulating paper degree of aging.
Description
Technical field
The present invention relates to electric device maintenance technical field, the detection of concentration of alcohol in especially a kind of transformer insulation oil
Method and its application in terms of determining power transformer Aging of Oil-paper Insulation in Oil.
Background technique
Power transformer is the key that realize voltage class transformation and electric energy transmission, is to ensure power network safety operation
One of most crucial equipment.In the power system, oil-immersed power transformer is due to having good insulation performance and longer
Service life, therefore be commonly utilized in the power transmission and transformation system of voltage levels.Oil-paper insulation combination is used as oil immersed type transformation
Main insulating forms inside device, as the long-play of transformer can be subjected to mechanical stress, moisture, electric field, temperature etc. respectively
The influence of kind factor, and synergistic effect can be also generated between various factors, it is common to accelerate oil-paper insulated deterioration, to lead
The insulation performance of mutagens depressor gradually fails, and becomes the main reason for causing transformer to break down.Insulating paper is as transformer
Solid dielectric insulation in oil-paper insulation system, for insulating oil, the aging of insulating paper hardly results in reparation, so
Generally believe that the service life of insulating paper determines the service life of transformer, if the aging of insulating paper will likely seriously will lead to change
Great electric power accident occurs for depressor, so just seeming most important for the accurate evaluation of insulating paper ageing state.About exhausted
The assessment of edge paper ageing state can from two aspects, first is that directly surveying the degree of polymerization of insulating paper, that is, DP value；Second is that logical
The aging character product of survey insulating paper is crossed to characterize insulating paper degree of aging.However the measurement of DP value is currently a big difficulty, because
To need power failure operation and suspended core sampling must be carried out to transformer, apply at the scene highly difficult.Therefore it is used in engineering
The assessment that the method carries out transformer interior insulation paper degree of aging is unsatisfactory.Therefore, some researchers set about with CO,
CO2The ageing state and fault type that transformer insulating paper is characterized Deng the gas that dissolves in oil, achieve great successes, but
Characteristic gas especially low molecular hydrocarbon mostlys come from the cracking of insulating oil in oil, not with the degree of aging relationship of insulating paper
Greatly.Then scholar starts to explore in oily furfural content to characterize the paper insulated ageing state of transformer, and in laboratory
A series of achievements are achieved under environment.However a large amount of transformers actual measurements experience have shown that, due to the influence vulnerable to various service conditions,
In oil furfural content with operation hours change dispersibility very greatly, even if use many modification methods, reflection paper it is exhausted
The accuracy of edge degree of aging can not show a candle to the ideal of the effect under laboratory condition, therefore limit the effective of its method to a certain extent
Using.Dependent on the development of gas-chromatography and mass spectrum detection, until in recent years, Jalbert etc. divides in laboratory conditions
From and identify more than 30 products of insulating paper aging, and have found methanol in the product, this is found to be insulating paper aging
Assessment new feature quantifier elimination provides new approaches.But methanol belongs to volatile gas, and this is the discovery that in laboratory condition
Lower progress in practice and is not suitable in engineering.
Therefore, we need to find effective new feature amount to characterize electric power transformer insulated paper degree of aging.For becoming
Depressor Aging of Oil-paper Insulation in Oil assesses the research and solution of this problem of new feature amount, and it is old that characterization transformer paper insulation not only can be improved
The accuracy of change or a kind of nondestructive evaluation means of achievable electrification sample detection, can be obviously improved the insulation fortune of transformer
Row maintenance levels has important theoretical academic significance and engineering practical value.
Summary of the invention
The invention discloses the detection methods and its application of concentration of alcohol in a kind of transformer insulation oil, are the old of insulating paper
The assessment of change degree provides a kind of new means.
To achieve the above object, the technical solution of the present invention is as follows:
The detection method of concentration of alcohol in a kind of transformer insulation oil, comprising the following steps:
S1. the preparation of reference substance solution: DMSO constant volume is added in ethyl alcohol standard items, and reference substance solution is made；
S2. it the preparation of test solution: the preparation of test solution: takes transformer insulation oil that container is added and is put into 0 DEG C
In following low temperature environment, while the container for filling DMSO being taken to be put into 0 DEG C or less low temperature environment, according to transformation under identical environment
Device insulating oil and DMSO volume ratio 1~4:1~4 are mixed in container, interval concussion 4~8 times, and interval, which is vortexed, to be mixed, concussion
After take supernatant, be centrifuged, take supernatant to cross film after centrifugation, obtain test solution；
S3. reference substance solution and test solution are detected respectively using gas-chromatography and mass spectrometry, is become
Concentration of alcohol in depressor insulating oil.
Further, GC conditions are as follows: 45 DEG C of post case temperature, carrier gas: He gas, flow rate of carrier gas 1.26mL/min, gas
Change 250 DEG C of room temperature, purge flow rate 3.0mL/min, column model: DN-1MS, 30m × 0.25mm × 0.25 μm；
Mass Spectrometry Conditions are as follows: electron impact ion source: the source EI, ion source temperature is 200.0 DEG C, 250.0 DEG C of interface temperature, electric
Ionization voltage is 70eV.
Wherein, DMSO is dimethyl sulfoxide.
The detection method that the present invention still further provides concentration of alcohol in transformer insulation oil is determining power transformer
Application in terms of Aging of Oil-paper Insulation in Oil.
Whether detection method of the invention, operation is fast and convenient, and detection speed is fast, can quickly analyze in insulating oil and contain
Alcohol component, to help quickly to determine the paper insulated ageing state of power transformer.
Detection method through the invention can successfully be detected alcohol component from the insulation oil samples of old transformer,
And methanol and furfural both ingredients are not but gone out in insulating oil sample detection using identical method, it was demonstrated that ethyl alcohol can be made
For a kind of new feature amount of Efficient Characterization transformer insulating paper aging, and, invention higher compared to methanol and furfural reliability
Has many advantages, such as lossless, easy, portable.And the influence due to furfural vulnerable to various service conditions, methanol belong to effumability
Gas, so the ageing state for using ethyl alcohol as new feature amount to characterize transformer insulating paper has more extensively in realistic meaning
General applicability compensates for the deficiency based on dielectric and traditional physico-chemical method, can apply to field diagnostic, compared to other agings
Appraisal procedure dependable with function is higher.
The present invention provides a kind of new feature amount for oil-immersed power transformer Aging of Oil-paper Insulation in Oil status assessment, it may be said that is
The Aging Assessment of insulating paper opens a kind of new thinking.Compared to the appraisal procedure of other characteristic quantities, the present invention is as a kind of
New thinking, advantages and features become apparent.
Detailed description of the invention
Fig. 1 a is the TIC chromatogram of ethyl alcohol standard solution (reference substance), and Fig. 1 b is the mesh of ethyl alcohol standard solution (reference substance)
Mark constitutional diagram.
Fig. 2 a is the TIC chromatogram of 1# insulation oil samples (DMSO extraction), and Fig. 2 b is 1# insulation oil samples (DMSO extraction)
Target components figure.
Fig. 3 a is the TIC chromatogram of 2# insulation oil samples (DMSO extraction), and Fig. 3 b is 2# insulation oil samples (DMSO extraction)
Target components figure.
Fig. 4 a is the TIC chromatogram of 3#, 4# insulation oil samples (DMSO extraction), and Fig. 4 b is 3#, 4# insulation oil samples (DMSO
Extraction) target components figure.
Fig. 5 is the canonical plotting of ethyl alcohol.
Fig. 6 a is the TIC chromatogram of methanol standard solution, and Fig. 6 b is the target components figure of methanol standard solution.
Fig. 7 a is the TIC chromatogram of 1# insulating oil methanol mark-on product (DMSO extraction), and Fig. 7 b is 1# insulating oil methanol mark-on
The target components figure of product (DMSO extraction).
Fig. 8 a is the TIC chromatogram of 2# insulating oil methanol mark-on product (DMSO extraction), and Fig. 8 b is 2# insulating oil methanol mark-on
The target components figure of product (DMSO extraction).
Fig. 9 a is the TIC chromatogram of furfural standard solution, and Fig. 9 b is the target components figure of furfural standard solution.
Figure 10 is the TIC chromatogram of 1# insulation oil samples (acetonitrile extraction).
Figure 11 is the target components figure of 2# insulation oil samples (acetonitrile extraction).
Figure 12 a is the TIC chromatogram of 1# insulating oil furfural mark-on product (acetonitrile extraction), and Figure 12 b is that 1# insulating oil furfural adds
The target components figure of mark product (acetonitrile extraction).
Figure 13 a is the TIC chromatogram of 2# insulating oil furfural mark-on product (acetonitrile extraction), and Figure 13 b is that 2# insulating oil furfural adds
The target components figure of mark product (acetonitrile extraction).
Specific embodiment
Below in conjunction with specific embodiment, the invention will be further described, but protection scope of the present invention is not limited to following reality
Apply example.
The 220kV electricity of take two difference actual motions nearly 31 years (in July, 1987 puts into operation) and 26 years (in April, 1992 puts into operation)
Press the 1# insulation oil samples and 2# insulation oil samples of grade；Two are taken to be separately operable nearly 4 years (in April, 2014 puts into operation) and 6 years again
The 3# insulation oil samples and 4# insulation oil samples of the 220kV voltage class of (in May, 2012 puts into operation), Lai Jinhang power transformer paper
The assessment of insulation ag(e)ing state is verified.
1, the preparation of standard solution and testing sample solution:
The production of 1-1. furfural standard solution:
10 μ L furfural mark product are taken, the acetonitrile of 990 μ L is added, 100 times of furfural standard solution must be diluted；After 1# processing
Sample and 2# treated sample mark-on and diluted the measurement of film sample introduction.
The production of 1-2. methanol standard solution:
The methanol mark product of 15 μ L are taken, the DMSO of 1485 μ L is added, concussion mixes, and must dilute 100 times of methanol standard solution；
For 1#DSMO treated sample to be tested and 2#DSMO treated sample to be tested mark-on and diluted the measurement of film sample introduction.
The production of 1-3. ethyl alcohol standard solution (reference substance):
The ethyl alcohol mark product for taking 100 μ L add the DMSO of 900 μ L, and concussion mixes, and obtain No. 1 ethyl alcohol standard solution i.e.
100000ppm；And to No. 1 ethyl alcohol standard solution carry out dilution step by step obtain 10000ppm, 1000ppm, 500ppm, 250ppm,
The ethyl alcohol standard solution of 50ppm and 10ppm, wherein 10ppm, 50ppm, 250ppm, 500ppm and 1000ppm cross the measurement of film sample introduction
Standard curve, 1000ppm standard solution are also used to 1#DSMO treated sample and 2#DSMO treated sample mark-on.
The production of 1-4. insulation oil samples (acetonitrile extraction):
The centrifuge tube for filling 1#, 2#, 3# and 4# insulation oil samples is respectively put into ice in advance, and fills 4mL's for 4
The centrifuge tube of acetonitrile is put into ice, on ice by 1#, 2#, 3# and 4# insulation oil samples take respectively 4mL be put into fill acetonitrile from
In heart pipe, interval concussion 6 times, interval centrifuge tube is inserted into ice, after concussion, takes supernatant in centrifuge tube, with
The revolving speed of 10000rpm is centrifuged 5min, takes supernatant, and the supernatant of 1#, 2# insulation oil samples is respectively used to furfural mark-on and directly
Film sample introduction is crossed, directly cross film is respectively 1# insulation oil samples (acetonitrile extraction), 2# insulation oil samples (acetonitrile extraction), and furfural adds
Target is respectively 1# insulating oil furfural mark-on product, 2# insulating oil furfural mark-on product, the direct mistake of supernatant of 3#, 4# insulation oil samples
Film sample introduction, respectively 3# insulate oil samples (acetonitrile extraction), 4# insulation oil samples (acetonitrile extraction), the above sample for furfural at
That divides searches library detection.
The production of 1-5. insulation oil samples (DMSO extraction) (test solution):
The centrifuge tube for filling 1#, 2#, 3# and 4# insulation oil samples is respectively put into ice in advance, and fills 4mL's for 4
The centrifuge tube of DMSO is put into ice, on ice by 1#, 2#, 3# and 4# insulation oil samples take respectively 4mL be put into fill DMSO from
In heart pipe, interval concussion 6 times, interval, which is vortexed, to be mixed, and after concussion, supernatant is taken to turn in centrifuge tube with 10000rpm
Speed centrifugation 5min, takes supernatant, and the supernatant of 1#, 2# insulation oil samples is respectively used to the mark-on and direct film excessively of methanol, ethyl alcohol
Sample introduction, directly cross film is respectively 1# insulation oil samples (DMSO extraction), 2# insulation oil samples (DMSO extraction), methanol, ethyl alcohol
Mark-on is respectively 1# insulating oil first/ethyl alcohol mark-on product, 2# insulating oil first/ethyl alcohol mark-on product, the supernatant of 3#, 4# insulation oil samples
Liquid directly crosses film sample introduction, and respectively 3# insulate oil samples (DMSO extraction), 4# insulate oil samples (DMSO extraction), and the above sample is used
In the detection of methanol and ethyl alcohol, wherein methanol only make it is qualitative search library detection, and the ethyl alcohol in the oil samples that insulate then combines chromatogram
Carry out its concentration of further quantitative analysis.
2, step 1 make sample in ethyl alcohol, methanol and furfural content detection:
The determination of 2-1. chromatographic condition:
The determination of 2-1-1 GC conditions:
1 GC conditions of table
Column model: DN-1MS (30m × 0.25mm × 0.25 μm), injector temperature: 150 DEG C, carrier gas: He gas, into
Sample amount: input mode: 1.35ml crosses film sample injection.
The determination of 2-1-2 Mass Spectrometry Conditions:
Table 2 measures Mass Spectrometry Conditions when furfural
Table 3 measures Mass Spectrometry Conditions when methanol and ethyl alcohol
Electron impact ion source is the source EI, ionization voltage: 70eV.
The detection of 2-2. ethyl alcohol and methanol content:
It insulate respectively to methanol standard solution, ethyl alcohol standard solution, 1# first according to the Mass Spectrometry Conditions and chromatographic condition of 2-1
Oil samples (DMSO extraction), 2# insulation oil samples (DMSO extraction), 3# insulation oil samples (DMSO extraction), 4# insulation oil samples
(DMSO extraction), 1# insulating oil first/ethyl alcohol mark-on product, 2# insulating oil first/ethyl alcohol mark-on product carry out ethyl alcohol, methanol content is searched
Library.
(1) ethyl alcohol detects: not searching library to alcohol component in 3# and 4# insulation oil samples, the two map is identical, sees
Fig. 4.On the contrary, successfully being searched in ethyl alcohol standard solution, 1# insulation oil samples (DMSO extraction), 2# insulation oil samples (DMSO extraction)
Alcohol component has been arrived in library, and can obtain concentration of alcohol in 1#, 2# insulation oil samples in conjunction with chromatogram, and testing result is shown in Fig. 1, figure
2 and Fig. 3.
The relative standard deviation (RSD) being repeatedly measured in parallel is 2.3%, and exhausted by Comprehensive Comparison 1#, 2#
Edge oil samples (DMSO extraction) chromatogram is it is found that the peak area of 1# insulation oil samples is the peak face of 149146,2# insulation oil samples
Product is 147823.3.The relationship that peak area and concentration of alcohol can be obtained by the canonical plotting (see Fig. 5) of ethyl alcohol is y=3437.7x-
64376, wherein ordinate y indicates that peak area, abscissa x indicate concentration of alcohol (ppm).Therefore, by 1# insulating oil sample peak face
Product 149146,2# insulating oil sample peak area 147823.3 substitute into the insulation oil samples concentration of alcohol of above-mentioned relation Shi Ke get: 1#
62.112ppm, 2# insulate oil samples concentration of alcohol for 61.727ppm.
(2) methanol detects: the chromatogram of methanol standard solution is shown in Fig. 6 a, and the characteristic peak retention time of methanol is
1.505min, while it is carried out to search library, as shown in Figure 6 b, it was demonstrated that there are methanol contents.In conjunction with shown in Fig. 2 a and Fig. 3 a, 1#,
There is not methanol characteristic peak at 1.505min in the chromatogram of 2# insulation oil samples (DMSO extraction), i.e., does not detect methanol
Ingredient equally carries out it to search library, does not obtain the match information with methanol.
1# insulating oil methanol mark-on product are detected, chromatogram is as shown in Figure 7a, and retention time is 1.505min appearance
Methanol characteristic peak, while it is carried out to search library, as shown in Figure 7b, methanol information can be matched to.To 2# insulating oil methanol mark-on product
It being detected, chromatogram is as shown in Figure 8 a, and retention time is that methanol characteristic peak occurs in 1.505min, while carrying out searching library to it,
As shown in Figure 8 b, methanol information can be matched to.Through detecting, insulate oil samples in methanol in makings under the conditions of be not detected, but
The sample of standard items and mark-on has apparent methanol chromatographic peak and matched mass spectrogram, it was demonstrated that the inspection is reliable.
The detection of 2-3 furfural ingredient:
To furfural standard solution, 1# insulation oil samples (acetonitrile extraction), 2# insulation oil samples (acetonitrile extraction), 3# insulating oil
Sample (acetonitrile extraction), 4# insulation oil samples (acetonitrile extraction), 1# insulating oil furfural mark-on product, 2# insulating oil furfural mark-on product into
Row furfural ingredient searches library detection, and analysis whether there is furfural substance in test product.
Furfural standard solution is detected, the chromatogram of furfural standard solution as illustrated in fig. 9, protect by the characteristic peak of furfural
Staying the time is 5.181min, while carrying out searching library to it, as shown in figure 9b, searches out furfural ingredient.In conjunction with shown in Figure 10, Figure 11,
There is not furfural characteristic peak in 5.171min in the chromatogram of 1#, 2# insulation oil samples (acetonitrile extraction).
1# insulating oil furfural mark-on product are detected, as figure 12 a shows, retention time is 5.181min appearance to chromatogram
Furfural characteristic peak, while it is carried out to search library, as shown in Figure 12b, furfural information can be matched to.To 2# insulating oil furfural mark-on product
It being detected, as depicted in fig. 13 a, retention time is that furfural characteristic peak occurs in 5.201min, while carrying out searching library to it to chromatogram,
As illustrated in fig. 13b, furfural information can be matched to.Through detecting, insulate oil samples in furfural in makings under the conditions of be not detected, but
The sample of standard items and mark-on has apparent furfural chromatographic peak and matched mass spectrogram, it was demonstrated that the inspection is reliable.
Each test product ingredient of 2-4 searches library testing result:
Testing result is shown in Table 4:
4 insulating oil sample composition of table searches library testing result
2-5 interpretation of result:
Alcohol component is detected in the insulation oil samples of two old transformers of 1# and 2#, but is thrown in 3# and 4# two
Alcohol component is not detected in the new transformer insulated oil samples of fortune soon.Therefore it can obtain, ethyl alcohol can be used as assessment transformation
The new feature amount of device Aging of Oil-paper Insulation in Oil state.And the content of ethyl alcohol is greater than the exhausted of 2# transformer in the insulation oil samples of 1# transformer
Edge oil samples, it is seen then that how much the content of ethyl alcohol can be used as the standard for determining transformer Aging of Oil-paper Insulation in Oil degree.
Methanol and furfural both ingredients are not detected in insulation oil samples, it was demonstrated that ethyl alcohol can be used as a kind of effective table
The new feature amount of transformer insulating paper aging is levied, and higher compared to methanol and furfural reliability, invention has lossless, simple
Just, the advantages that portable.And the influence due to furfural vulnerable to various service conditions, methanol belong to effumability gas, so
In realistic meaning, the ageing state for using ethyl alcohol as new feature amount to characterize transformer insulating paper has wider applicability,
The deficiency based on dielectric and traditional physico-chemical method is compensated for, can apply to field diagnostic, it can compared to other aging assessments
It is higher by property and practicability.
Claims (3)
1. the detection method of concentration of alcohol in a kind of transformer insulation oil, it is characterised in that the following steps are included:
S1. the preparation of reference substance solution: DMSO constant volume is added in ethyl alcohol standard items, and reference substance solution is made；
S2. it the preparation of test solution: takes transformer insulation oil that container is added and is put into 0 DEG C or less low temperature environment, take simultaneously
The container for filling DMSO is put into 0 DEG C or less low temperature environment, according to transformer insulation oil and DMSO volume ratio 1 under identical environment
~4:1~4 are mixed in container, interval concussion 4~8 times, and interval, which is vortexed, to be mixed, and supernatant is taken after concussion, is centrifuged, from
It takes supernatant to cross film after the heart, obtains test solution；
S3. reference substance solution and test solution are detected respectively using gas-chromatography and mass spectrometry, obtains transformer
Concentration of alcohol in insulating oil.
2. the detection method of concentration of alcohol in transformer insulation oil according to claim 1, it is characterised in that:
GC conditions are as follows: 45 DEG C of post case temperature, carrier gas: He gas, flow rate of carrier gas 1.26mL/min gasify 250 DEG C of room temperature,
Purge flow rate 3.0mL/min, column model: DN-1MS, 30m × 0.25mm × 0.25 μm；
Mass Spectrometry Conditions are as follows: electron impact ion source: the source EI, ion source temperature are 200.0 DEG C, and 250.0 DEG C of interface temperature, ionization is electric
Pressure is 70eV.
3. the detection method of concentration of alcohol is determining power transformer paper in transformer insulation oil as claimed in claim 1 or 2
Application in terms of insulation ag(e)ing.
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| CN115201388A (en) * | 2022-08-01 | 2022-10-18 | 哈尔滨理工大学 | Intelligent sampling analysis system and sampling analysis method for methanol in transformer oil |
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Application publication date: 20190524 |