CN107796888A - Can accurate test transformer insulating oil furfural content method and its device - Google Patents
Can accurate test transformer insulating oil furfural content method and its device Download PDFInfo
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- CN107796888A CN107796888A CN201710925059.5A CN201710925059A CN107796888A CN 107796888 A CN107796888 A CN 107796888A CN 201710925059 A CN201710925059 A CN 201710925059A CN 107796888 A CN107796888 A CN 107796888A
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- furfural
- transformer
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- quantitative loop
- furfural content
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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
Abstract
The invention discloses it is a kind of can accurate test transformer insulating oil furfural content method and its device, solve the problems, such as the accurate test of the furfural content of transformer insulation oil.15 milliliters of transformer insulation oil is taken, takes 3 milliliters of methanol solution, after concussion mixes, is filtered, the extraction solution of accurate 60 microlitres of interception；By pump respectively by 60% methanol solution and 40% pure water, it is injected into quantitative loop sampler, then, 60 microlitres of extraction solution is injected into quantitative loop sampler, starts to test, test result is modified with empirical coefficient；After the completion of test, clear water is pumped into liquid phase furfural chromatographic column and cleaned, test and clean the same test container path of utilization.The test data of the furfural degree of aging of accurate transformer insulation oil has been provided for transformer station high-voltage side bus scene, ensure that the normal operation of transformer.
Description
Technical field
The present invention relates to a kind of furfural degradation of transformer insulation oil, more particularly to a kind of transformer insulation oil furfural
The method and its device of aging content.
Background technology
Transformer station high-voltage side bus in power system for many years after, insulating paper therein is after long-time heating, it may appear that loses
The aging phenomenon such as elasticity and mechanical strength decline.Judge the most reliable method of papery insulation ag(e)ing, be to determine its anti-tensile first
Intensity, next to that its degree of polymerization is determined, but all there is the problem of sampling is difficult in both approaches, only becoming for transformer
When cover is hung in depressor overhaul, above-mentioned sampling could be carried out and completed.For such case, now begin to employ a kind of more practicality
Transformer Aging of Oil-paper Insulation in Oil method of discrimination, i.e. high performance liquid chromatography（HPLC）Furfural content analytic approach, to differentiate transformer paper
Matter insulation ag(e)ing degree and its insulation life.The furfurol test method of existing transformer insulation oil mainly has high performance liquid chromatography
Two kinds of method and AAS, high performance liquid chromatography therein have the characteristics of measuring accuracy high and favorable reproducibility, but by
The characteristics of viscosity is high be present in transformer insulation oil, test container blocking is easily caused in test process, seriously constrain existing
Testing efficiency, in addition, when the furfural content that test parameter is converted to transformer insulation oil also be present, conversion error is big
Defect.
The content of the invention
The invention provides it is a kind of can accurate test transformer insulating oil furfural content method and its device, solve change
The technical problem of the accurate test of the furfural content of depressor insulating oil.
The present invention is that solve above technical problem by the following technical programs：
The present general inventive concept is：15 milliliters of transformer insulation oil is taken, takes 3 milliliters of methanol solution, after concussion mixes, is entered
Row filtering, the extraction solution of accurate 60 microlitres of interception；By pump respectively by 60% methanol solution and 40% pure water, it is fixed to be injected into
Measure in ring sampler, then, 60 microlitres of extraction solution is injected into quantitative loop sampler, starts to test, by test result
It is modified with empirical coefficient；After the completion of test, clear water is pumped into liquid phase furfural chromatographic column and cleaned, tests and clean utilization
Same test container path.
It is a kind of can accurate test transformer insulating oil furfural content method, it is characterised in that following steps：
The first step, 3 milliliters of 15 milliliters of transformer insulation oil and methanol solution are taken with needle tubing, be injected into triangle cup, and stopper mill
Sand lid；It it is 280 beats/min with frequency of oscillation, amplitude is 30 millimeters of triangle cup shaker, and the triangle cup for injecting solution is carried out
Vibration, time are 20 minutes；Now, the ratio of the methanol solution of extractant and transformer insulation oil is 3/15；
Second step, the solvent after vibration stood 5 minutes, then with extractant is obtained after molecular filtration sieve mouth filtering, and filled
Enter sample to prevent putting in bottle；
3rd step, by methanol solution pure water according to 3：2 ratio is driven into the quantitative loop injector of furfural content verifying attachment；
4th step, from sample anti-put 60 microlitres of extractant is taken in bottle, be injected into quantitative loop injector, tested, obtained
To the measure numerical value a of high performance liquid chromatography furfural content instrument；
5th step, measure numerical value a is first multiplied by the methanol solution of extractant and the ratio 3/15 of transformer insulation oil, then divided by
Furfural content in the numerical value obtained after correction value 0.72, as transformer insulation oil.
It is a kind of realize can accurate test transformer insulating oil furfural content method testing device, including liquid phase furfural color
Post and the injector with quantitative loop are composed, is respectively arranged with the injection port of the injector with quantitative loop and methanol solution bottle
The methanol solution pressure liquid pump of connection, the pure water solution pressure liquid pump connected with pure water solution bottle and transformer insulation oil first
Alcohol extraction solution injection needle tubing；The injector outlet of quantitative loop passes through sample introduction triple valve and the injection port of liquid phase furfural chromatographic column
Connection, the outlet of liquid phase furfural chromatographic column are connected by going out sample triple valve with ultraviolet spectra calibrating instrument.
The 3rd waste liquid recovery apparatus is connected with ultraviolet spectra calibrating instrument, first is connected with the injector of quantitative loop
Waste liquid recovery apparatus, the second waste liquid recovery apparatus is connected with sample introduction triple valve.
The present invention realizes the common channel loop of test and cleaning by double pump, has reached after testing to liquid phase furfural chromatogram
The timely cleaning of post, and by the extracted by filtration to insulating oil, greatly reduce the blocking wind of the test container in test process
Danger, the ratio of the insulating oil and methanol solution according to extraction solution is found out especially by many experiments, to measuring data
Accurate amendment, for transformer station high-voltage side bus scene provided accurate transformer insulation oil furfural degree of aging test number
According to ensure that the normal operation of transformer.
Brief description of the drawings
Fig. 1 is apparatus structure schematic diagram of the present invention in test；
Fig. 2 is apparatus structure schematic diagram of the present invention when cleaning liquid phase furfural chromatographic column.
Embodiment
The present invention is described in detail below in conjunction with the accompanying drawings：
It is a kind of can accurate test transformer insulating oil furfural content method, it is characterised in that following steps：
The first step, 3 milliliters of 15 milliliters of transformer insulation oil and methanol solution are taken with needle tubing, be injected into triangle cup, and stopper mill
Sand lid；It it is 280 beats/min with frequency of oscillation, amplitude is 30 millimeters of triangle cup shaker, and the triangle cup for injecting solution is carried out
Vibration, time are 20 minutes；Now, the ratio of the methanol solution of extractant and transformer insulation oil is 3/15；
Second step, the solvent after vibration stood 5 minutes, then with extractant is obtained after molecular filtration sieve mouth filtering, and filled
Enter sample to prevent putting in bottle；
3rd step, by methanol solution pure water according to 3：2 ratio is driven into the quantitative loop injector of furfural content verifying attachment（5）
In；
4th step, from sample anti-put 60 microlitres of extractant is taken in bottle, be injected into quantitative loop injector 5, tested, obtained
To the measure numerical value a of high performance liquid chromatography furfural content instrument；
5th step, measure numerical value a is first multiplied by the methanol solution of extractant and the ratio 3/15 of transformer insulation oil, then divided by
Furfural content in the numerical value obtained after correction value 0.72, as transformer insulation oil；Because obtained result is done in this experiment
For furfural aging content contained in transformer oil, and detected by instrument for the furfural content that extracts, so needs pair
Testing result is modified.
It is a kind of realize can accurate test transformer insulating oil furfural content method testing device, including liquid phase furfural color
Post 9 and the injector 5 with quantitative loop are composed, is respectively arranged with the injection port of the injector 5 with quantitative loop molten with methanol
The methanol solution pressure liquid pump 1 of the connection of liquid bottle 2, the pure water solution pressure liquid pump 3 and transformer connected with pure water solution bottle 4
Insulating oil methanol extraction solution injects needle tubing；The outlet of injector 5 with quantitative loop passes through sample introduction triple valve 7 and liquid phase furfural
The injection port connection of chromatographic column 9, the outlet of liquid phase furfural chromatographic column 9 is by going out sample triple valve 8 and ultraviolet spectra calibrating instrument 11
Connection.
The 3rd waste liquid recovery apparatus 12 is connected with ultraviolet spectra calibrating instrument 11, on the injector 5 with quantitative loop
The first waste liquid recovery apparatus 6 is connected with, the second waste liquid recovery apparatus 10 is connected with sample introduction triple valve 7.
Methanol solution pressure liquid pump 1 is connected with methanol solution bottle 2, pure water solution pressure liquid pump 3 and pure water solution bottle 4
It is connected, by the function of pump, methanol solution and pure water solution is blended to the entering with quantitative loop for squeezing into furfural sampling device
In sample device 5.By the extraction to insulating oil, the solvent of furfural content is extracted, takes the extractant injection more than 60ul capacity
Into the injector 5 with quantitative loop, the accurate extractant for intercepting 60ml, remaining solvent will go into the first devil liquor recovery dress
Put in 6.The 60ml extractants that are intercepted are entered in detection means with methanol and pure water, sample introduction triple valve 7 and go out sample threeway
The state of valve 8 is measuring state, and extraction solution enters directly into liquid phase furfural chromatographic column 9 and separated, with automatic shutter work(
Second waste liquid recovery apparatus 10 of energy belongs to closed mode, subsequently enters and content detection is carried out in ultraviolet spectra calibrating instrument 11, most
Waste liquid is flowed into the 3rd waste liquid recovery apparatus 12 afterwards.
If liquid phase furfural chromatographic column 9 is found that clogging, sample introduction triple valve 7 becomes thin with the state for going out sample triple valve 8
Logical chromatographic column state, triple valve 7 is connected with going out sample triple valve 8, the second devil liquor recovery dress with automatic shutter function
It is opening to put 10, and methanol solution pressure liquid pump 1 is stopped, and pure water solution pressure liquid pump 3 individually opens work, enters
Liquid phase furfural chromatographic column 9 can be dredged for 10 minutes by entering to dredging chromatographic column state, such continuous firing.
Claims (3)
1. it is a kind of can accurate test transformer insulating oil furfural content method, it is characterised in that following steps：
The first step, 3 milliliters of 15 milliliters of transformer insulation oil and methanol solution are taken with needle tubing, be injected into triangle cup, and stopper mill
Sand lid；It it is 280 beats/min with frequency of oscillation, amplitude is 30 millimeters of triangle cup shaker, and the triangle cup for injecting solution is carried out
Vibration, time are 20 minutes；Now, the ratio of the methanol solution of extractant and transformer insulation oil is 3/15；
Second step, the solvent after vibration stood 5 minutes, then with extractant is obtained after molecular filtration sieve mouth filtering, and filled
Enter sample to prevent putting in bottle；
3rd step, by methanol solution pure water according to 3：2 ratio is driven into the quantitative loop injector of furfural content verifying attachment（5）
In；
4th step, from sample anti-put 60 microlitres of extractant is taken in bottle, be injected into quantitative loop injector（5）In, tested,
Obtain the measure numerical value a of high performance liquid chromatography furfural content instrument；
5th step, measure numerical value a is first multiplied by the methanol solution of extractant and the ratio 3/15 of transformer insulation oil, then divided by
Furfural content in the numerical value obtained after correction value 0.72, as transformer insulation oil.
2. it is a kind of realize can accurate test transformer insulating oil furfural content method testing device, including liquid phase furfural chromatogram
Post（9）With the injector with quantitative loop（5）, in the injector with quantitative loop（5）Injection port on be respectively arranged with and first
Alcoholic solution bottle（2）The methanol solution pressure liquid pump of connection（1）And pure water solution bottle（4）The pure water solution highly pressurised liquid of connection
Pump（3）Needle tubing is injected with transformer insulation oil methanol extraction solution；The injector of quantitative loop（5）Outlet passes through sample introduction triple valve
（7）With liquid phase furfural chromatographic column（9）Injection port connection, liquid phase furfural chromatographic column（9）Outlet by going out sample triple valve（8）
With ultraviolet spectra calibrating instrument（11）Connection.
3. it is according to claim 1 it is a kind of realize can accurately test transformer insulating oil furfural content method testing dress
Put, it is characterised in that in ultraviolet spectra calibrating instrument（11）On be connected with the 3rd waste liquid recovery apparatus（12）, in the sample introduction of quantitative loop
Device（5）On be connected with the first waste liquid recovery apparatus（6）, in sample introduction triple valve（7）On be connected with the second waste liquid recovery apparatus（10）.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710925059.5A CN107796888A (en) | 2017-10-02 | 2017-10-02 | Can accurate test transformer insulating oil furfural content method and its device |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710925059.5A CN107796888A (en) | 2017-10-02 | 2017-10-02 | Can accurate test transformer insulating oil furfural content method and its device |
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| Publication Number | Publication Date |
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| CN107796888A true CN107796888A (en) | 2018-03-13 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201710925059.5A Withdrawn CN107796888A (en) | 2017-10-02 | 2017-10-02 | Can accurate test transformer insulating oil furfural content method and its device |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102175795A (en) * | 2011-01-16 | 2011-09-07 | 青海电力科学试验研究院 | Method for calculating furfural component in shake extraction test oil |
| CN104007192A (en) * | 2014-05-08 | 2014-08-27 | 广东电网公司电力科学研究院 | Determination method for metal deactivator, furfural and anti-oxidant in insulating oil |
| CN104730184A (en) * | 2013-12-18 | 2015-06-24 | 上海宝钢工业技术服务有限公司 | Method for determining content of furfural and furan derivative in insulating oil |
-
2017
- 2017-10-02 CN CN201710925059.5A patent/CN107796888A/en not_active Withdrawn
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102175795A (en) * | 2011-01-16 | 2011-09-07 | 青海电力科学试验研究院 | Method for calculating furfural component in shake extraction test oil |
| CN104730184A (en) * | 2013-12-18 | 2015-06-24 | 上海宝钢工业技术服务有限公司 | Method for determining content of furfural and furan derivative in insulating oil |
| CN104007192A (en) * | 2014-05-08 | 2014-08-27 | 广东电网公司电力科学研究院 | Determination method for metal deactivator, furfural and anti-oxidant in insulating oil |
Non-Patent Citations (1)
| Title |
|---|
| 国家能源局: "DL/T1355-2014 变压器油中糠醛含量的测定", 《中华人民共和国电力行业标准》 * |
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Application publication date: 20180313 |
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