CN103954520B - A kind of method detecting active sulfur content in insulating oil - Google Patents
A kind of method detecting active sulfur content in insulating oil Download PDFInfo
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- CN103954520B CN103954520B CN201410172101.7A CN201410172101A CN103954520B CN 103954520 B CN103954520 B CN 103954520B CN 201410172101 A CN201410172101 A CN 201410172101A CN 103954520 B CN103954520 B CN 103954520B
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- 238000000034 method Methods 0.000 title claims abstract description 27
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 title claims abstract description 19
- 239000011593 sulfur Substances 0.000 title claims abstract description 19
- 229910052717 sulfur Inorganic materials 0.000 title claims abstract description 19
- 239000013078 crystal Substances 0.000 claims abstract description 61
- 239000010453 quartz Substances 0.000 claims abstract description 58
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 58
- 230000004913 activation Effects 0.000 claims abstract description 25
- 230000010287 polarization Effects 0.000 claims abstract description 25
- 230000008859 change Effects 0.000 claims abstract description 22
- 238000012360 testing method Methods 0.000 claims abstract description 18
- 239000011259 mixed solution Substances 0.000 claims abstract description 8
- -1 1-butyl-3-methylimidazole hexafluorophosphoric acid Chemical compound 0.000 claims abstract description 3
- 239000002608 ionic liquid Substances 0.000 claims abstract description 3
- 238000003380 quartz crystal microbalance Methods 0.000 claims description 39
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 12
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 6
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 6
- 229910052697 platinum Inorganic materials 0.000 claims description 6
- 230000002093 peripheral effect Effects 0.000 claims description 4
- 229910052709 silver Inorganic materials 0.000 claims description 4
- 239000004332 silver Substances 0.000 claims description 4
- 229910021607 Silver chloride Inorganic materials 0.000 claims description 3
- 238000010008 shearing Methods 0.000 claims description 3
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 claims description 3
- 229910052938 sodium sulfate Inorganic materials 0.000 claims description 3
- 235000011152 sodium sulphate Nutrition 0.000 claims description 3
- 239000000243 solution Substances 0.000 claims description 3
- 238000004832 voltammetry Methods 0.000 claims description 3
- 239000007864 aqueous solution Substances 0.000 claims description 2
- 238000000083 pulse voltammetry Methods 0.000 claims description 2
- 238000003745 diagnosis Methods 0.000 abstract description 2
- 230000008439 repair process Effects 0.000 abstract description 2
- 239000000523 sample Substances 0.000 abstract 2
- 238000004445 quantitative analysis Methods 0.000 abstract 1
- 239000012488 sample solution Substances 0.000 abstract 1
- 238000001514 detection method Methods 0.000 description 8
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000013519 translation Methods 0.000 description 3
- 230000007797 corrosion Effects 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- AQMRBJNRFUQADD-UHFFFAOYSA-N copper(I) sulfide Chemical compound [S-2].[Cu+].[Cu+] AQMRBJNRFUQADD-UHFFFAOYSA-N 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000000840 electrochemical analysis Methods 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000003209 petroleum derivative Substances 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 150000003568 thioethers Chemical class 0.000 description 1
Landscapes
- Testing Resistance To Weather, Investigating Materials By Mechanical Methods (AREA)
Abstract
Invention describes a kind of method detecting active sulfur content in insulating oil, comprise the steps: (1) to get insulating oil sample or insulating oil sample, 1-butyl-3-methylimidazole hexafluorophosphoric acid ionic liquid is mixed into transformer oil mixed solution; (2) sample or mixed solution are coated on Quartz crystal resonant sheet and are connected with testing workstation; (3) recording frequency f
1; (4) implement activation polarization test, recording frequency f
2; (5) press formula Δ f=f
1-f
2calculate frequency change Δ f; (6) use formula Δ f=-2f
0 2Δ m/A (μ
qρ
q)
1/2calculate the content of active sulfur in transformer insulating oil.This method energy accurate quantitative analysis detects the content of active sulfur in transformer oil, and device is simple, easy to operate, has very important directive significance for the Hidden fault of diagnosis transformer and repair based on condition of component work how to carry out transformer.
Description
Technical field
The present invention relates to a kind of method detecting oil property, especially a kind of method detecting active sulfur content in transformer insulating oil.
Background technology
The quality of transformer insulating oil performance is directly connected to safe operation and the serviceable life of electrical equipment.And the sulfide in transformer insulating oil, in transformer operational process, cuprous sulfide can be formed on insulating paper and corrosive attack is produced to copper coil.First this sulfide can make the insulating property of insulating paper reduce, and causes the insulating paper of transformer breakdown, thus it is damaged to cause transformer.So, strengthen the supervisory detection of active sulfur in insulating oil especially aobvious necessary.But, up to the present, in insulating oil the detection of active sulfur still adopt traditional ASTMD (wherein " ASTM " abbreviation that to be English full name be " AmericanSocietyforTestingandMaterials ", its Chinese translation is " American Society Testing and Materials "; " D " is Sort Code, means and comprises petroleum products, fuel, and low strong plastics are at the code of interior material.) 1275 quilitative methods, or IEC (English full name is the abbreviation of " InternationalElectrotechnicalCommission ", and its Chinese translation is " International Electrotechnical Commission ".) 62535 quilitative methods, (German full name is the abbreviation of " DeutschesInstitutf ü rNormunge.V. " to DIN, and its Chinese translation is " DIN chemistry meeting ".) 51353 quilitative methods, (wherein " GB " is the abbreviation of Chinese pinyin " GUOJIABIAOZHUN " to GB/T, and its Chinese is " national standard ", and " T " represents recommendation.) 25961 quilitative methods.These traditional quilitative method ubiquities above-mentioned length consuming time, inefficient defect.Such as the intuitive judgment to color is mainly relied on to the judgement of test findings, therefore cannot give quantificational description to the corrosive nature of oil product.In order to quantize to judge accurately to insulating oil corrosion condition, be extremely necessary to design a kind of method detecting active sulfur content in transformer insulating oil as early as possible, to provide safeguard for the safe operation of electrical equipment.
Summary of the invention
The technical problem to be solved in the present invention is, for the ubiquitous defect of detection method of active sulfur content in traditional transformer insulating oil, the method of active sulfur content in a kind of detection insulating oil of improvement is provided, require that needed for the method, detection time is short, efficiency is high, can quantize accurately to judge to insulating oil corrosion condition, thus can provide safeguard for the safe operation of electrical equipment.
Technical scheme of the present invention is, a kind of method detecting active sulfur content in insulating oil provided comprises following processing step:
(1) get and entrust transformer insulating oil sample used 0.05ml ~ 0.5ml; Or get entrust transformer insulating oil sample used 0.05ml ~ 0.5ml, 1-butyl-3-methylimidazole hexafluorophosphoric acid ionic liquid 0.05ml ~ 0.5ml or potassium hydroxide aqueous solution 0.05ml ~ 0.5ml or sodium sulphate ethanolic solution 0.05ml ~ 0.5ml is hybridly prepared into transformer oil mixed solution;
(2) get QCM (Quartz Crystal Microbalance) 1.By step (1) get entrust transformer insulating oil used sample or step (1) obtained transformer oil mixed solution even application on the Quartz crystal resonant sheet of got QCM (Quartz Crystal Microbalance).Then this Quartz crystal resonant sheet is inserted in the sensor stand of got QCM (Quartz Crystal Microbalance), and by wire, described Quartz crystal resonant sheet is connected with peripheral hardware electrochemical quartz crystal microbalance testing workstation.Use QCM (Quartz Crystal Microbalance) (QCM) detection limit can arrive nanogram level.Electrochemical techniques and QCM technical battery are used, set up into electrochemical quartz crystal microbalance (EQCM) technology, the information of quarts crystal electrode surface quality change can be obtained on the one hand by the detection of QCM frequency, quarts crystal electrode is as the working electrode of electro-chemical test system on the other hand, the measurement to electrochemical parameter can be realized, thus obtain the various information of electrode surface galvanochemistry and non-electrochemical process simultaneously; The QCM (Quartz Crystal Microbalance) (QCM) used in this step is the piezoelectric property utilizing quartz-crystal resonator, the frequency change change of quartz crystal oscillator electrode surface quality being converted into quartz crystal oscillator circuit output electric signal is measured, there is the advantages such as highly sensitive, equipment is simple, detectability can arrive nanogram level, the fields such as chemistry, physics, biology, medical science and material science are widely used in, but QCM technology is not applied to active sulfur detection field before this always, for people stay many sorry.
Recording step (2) in insert the frequency f of the Quartz crystal resonant sheet of described sensor stand
1;
Using described Quartz crystal resonant sheet as working electrode, platinum electrode is used to be the conventional three-electrode system that is contrast electrode to electrode, silver/silver chloride electrode to routine two electrode system of electrode or platinum electrode, with conventional potentiostatic method or conventional linear scanning method or conventional galvanostatic method or general pulse voltammetry or regular circulation voltammetry, activation polarization test is implemented to this Quartz crystal resonant sheet.When this Quartz crystal resonant sheet obtains activation polarization, record frequency f during this Quartz crystal resonant sheet acquisition activation polarization
2;
(5) according to formula Δ f=f
1-f
2, in formula, Δ f is frequency change, f
1for the frequency of Quartz crystal resonant sheet before activation polarization, f
2for the frequency of Quartz crystal resonant sheet after activation polarization, calculate step and (4) described Quartz crystal resonant sheet frequency change Δ f before and after activation polarization test is implemented to Quartz crystal resonant sheet;
(6) use formula Δ f=-2f
0 2Δ m/A (μ
qρ
q)
1/2, in formula, Δ f is frequency change, f
0for Quartz crystal resonant sheet fundamental frequency, Δ m is mass change, and A is the reaction area of Quartz crystal resonant sheet, μ
qfor modulus of shearing constant, ρ
qfor crystalline density, calculate step and (4) namely the quality of sulfur product is corroded to the mass change Δ m of described Quartz crystal resonant sheet before and after the test of Quartz crystal resonant sheet enforcement activation polarization, the value of this mass change Δ of gained m divided by step (1) get and entrust transformer insulating oil sample volume used, be the content of active sulfur in described trust transformer insulating oil used.
The invention has the beneficial effects as follows: the content that easily and accurately quantitatively can detect active sulfur in transformer oil, device is simple, easy to operate, for the Hidden fault of diagnosis transformer and repair based on condition of component work how to carry out transformer, there is very important directive significance.
Embodiment
Embodiment 1:
(1) get and entrust 220kV transformer insulating oil sample used 0.05ml;
(2) get commercially available two-sided by silver type QCM (Quartz Crystal Microbalance) 1.By step (1) get and entrust 220kV transformer insulating oil used sample even application on the Quartz crystal resonant sheet of got QCM (Quartz Crystal Microbalance).Then this Quartz crystal resonant sheet is inserted in the sensor stand of got QCM (Quartz Crystal Microbalance), and by wire, described Quartz crystal resonant sheet is connected with peripheral hardware electrochemical quartz crystal microbalance testing workstation;
Recording step (2) in insert the frequency f of the Quartz crystal resonant sheet of described sensor stand
1;
Using described Quartz crystal resonant sheet as working electrode, use conventional platinum electrode to be two electrode systems to electrode and conventional potentiostatic method, activation polarization test implemented to this Quartz crystal resonant sheet, current potential 1.5V.When this Quartz crystal resonant sheet obtains activation polarization, record frequency f during this Quartz crystal resonant sheet acquisition activation polarization
2;
(5) according to formula Δ f=f
1-f
2, in formula, Δ f is frequency change, f
1for the frequency of Quartz crystal resonant sheet before activation polarization, f
2for the frequency of Quartz crystal resonant sheet after activation polarization, calculate step and (4) described Quartz crystal resonant sheet frequency change Δ f before and after activation polarization test is implemented to Quartz crystal resonant sheet;
(6) use formula Δ f=-2f
0 2Δ m/A (μ
qρ
q)
1/2, in formula, Δ f is frequency change, f
0for Quartz crystal resonant sheet fundamental frequency, Δ m is mass change, and A is the reaction area of Quartz crystal resonant sheet, μ
qfor modulus of shearing constant, ρ
qfor crystalline density, calculate (4) step implements described Quartz crystal resonant sheet before and after activation polarization test mass change Δ m to Quartz crystal resonant sheet, the value of this mass change Δ of gained m divided by step (1) get and entrust transformer insulating oil sample volume used, be the content of entrusting active sulfur in transformer insulating oil used.
Embodiment 2:
(1) get and entrust 110kV transformer insulating oil sample used 0.5ml, sodium sulphate ethanolic solution 0.5ml is hybridly prepared into transformer oil mixed solution;
(2) get commercially available QCM type QCM (Quartz Crystal Microbalance) 1.By step (1) obtained transformer oil mixed solution even application on the Quartz crystal resonant sheet of got QCM (Quartz Crystal Microbalance).Then this Quartz crystal resonant sheet is inserted in the sensor stand of got QCM (Quartz Crystal Microbalance), and by wire, described Quartz crystal resonant sheet is connected with peripheral hardware electrochemical quartz crystal microbalance testing workstation;
Step is (3) with embodiment 1;
Using described Quartz crystal resonant sheet as working electrode, platinum electrode is used to be to electrode, silver/silver chloride electrode be contrast electrode conventional three-electrode system and regular circulation voltammetry, activation polarization test is implemented to this Quartz crystal resonant sheet, initial voltage-0.5V, final voltage 2.0V, sweep velocity 0.05V/s.When this Quartz crystal resonant sheet obtains activation polarization, record frequency f during this Quartz crystal resonant sheet acquisition activation polarization
2;
Step (5) ~ (6) with embodiment 1.
Claims (1)
1. detect a method for active sulfur content in insulating oil, the method comprises the steps:
(1) get and entrust transformer insulating oil sample used 0.05ml ~ 0.5ml; Or get entrust transformer insulating oil sample used 0.05ml ~ 0.5ml, 1-butyl-3-methylimidazole hexafluorophosphoric acid ionic liquid 0.05ml ~ 0.5ml or potassium hydroxide aqueous solution 0.05ml ~ 0.5ml or sodium sulphate ethanolic solution 0.05ml ~ 0.5ml is hybridly prepared into transformer oil mixed solution;
(2) get QCM (Quartz Crystal Microbalance) 1, by step (1) get entrust transformer insulating oil used sample or step (1) obtained transformer oil mixed solution even application on the Quartz crystal resonant sheet of got QCM (Quartz Crystal Microbalance), then this Quartz crystal resonant sheet is inserted in the sensor stand of got QCM (Quartz Crystal Microbalance), and by wire, described Quartz crystal resonant sheet is connected with peripheral hardware electrochemical quartz crystal microbalance testing workstation;
Recording step (2) in insert the frequency f of the Quartz crystal resonant sheet of described sensor stand
1;
Using described Quartz crystal resonant sheet as working electrode, platinum electrode is used to be the conventional three-electrode system that is contrast electrode to electrode, silver/silver chloride electrode to routine two electrode system of electrode or platinum electrode, with conventional potentiostatic method or conventional linear scanning method or conventional galvanostatic method or general pulse voltammetry or regular circulation voltammetry, activation polarization test is implemented to this Quartz crystal resonant sheet, when this Quartz crystal resonant sheet obtains activation polarization, record frequency f during this Quartz crystal resonant sheet acquisition activation polarization
2;
(5) according to formula Δ f=f
1-f
2, in formula, Δ f is frequency change, f
1for the frequency of Quartz crystal resonant sheet before activation polarization, f
2for the frequency of Quartz crystal resonant sheet after activation polarization, calculate step and (4) described Quartz crystal resonant sheet frequency change Δ f before and after activation polarization test is implemented to Quartz crystal resonant sheet;
(6) use formula Δ f=-2f
0 2Δ m/A (μ
qρ
q)
1/2, in formula, Δ f is frequency change, f
0for Quartz crystal resonant sheet fundamental frequency, Δ m is mass change, and A is the reaction area of Quartz crystal resonant sheet, μ
qfor modulus of shearing constant, ρ
qfor crystalline density, calculate (4) step implements described Quartz crystal resonant sheet before and after activation polarization test mass change Δ m to Quartz crystal resonant sheet, the value of this mass change Δ of gained m divided by step (1) get and entrust transformer insulating oil sample volume used, be the content of active sulfur in described trust transformer insulating oil used.
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| CN104807902B (en) * | 2015-04-27 | 2016-06-08 | 广东电网有限责任公司电力科学研究院 | The detection method of benzyldithio toluene and antioxidant in insulating oil |
| CN105092458A (en) * | 2015-08-13 | 2015-11-25 | 国家电网公司 | Method for evaluating sulfur corrosion state of transformer copper coil |
| CN105388227A (en) * | 2015-10-29 | 2016-03-09 | 山东中实易通集团有限公司 | Quantitative detection method of benzyl disulfide in oil in oil-filled electrical equipment oil |
| CN105181940B (en) * | 2015-10-29 | 2017-03-29 | 大庆市日上仪器制造有限公司 | A kind of explosion-proof automatic air-exchanging insulating oil active sulfur analyzer |
| CN108693223A (en) * | 2017-04-06 | 2018-10-23 | 北京至感传感器技术研究院有限公司 | The on-line monitoring method and system of active sulfur in liquid oil |
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