CN103954521B - Detect the method for active sulfur content in insulating oil - Google Patents
Detect the method for active sulfur content in insulating oil Download PDFInfo
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- CN103954521B CN103954521B CN201410172583.6A CN201410172583A CN103954521B CN 103954521 B CN103954521 B CN 103954521B CN 201410172583 A CN201410172583 A CN 201410172583A CN 103954521 B CN103954521 B CN 103954521B
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- quartz crystal
- resonant sheet
- constant temperature
- frequency
- crystal resonant
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- 238000000034 method Methods 0.000 title claims abstract description 24
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 title claims abstract description 19
- 229910052717 sulfur Inorganic materials 0.000 title claims abstract description 19
- 239000011593 sulfur Substances 0.000 title claims abstract description 19
- 239000013078 crystal Substances 0.000 claims abstract description 47
- 239000010453 quartz Substances 0.000 claims abstract description 44
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 44
- 230000008859 change Effects 0.000 claims abstract description 22
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 5
- 238000003380 quartz crystal microbalance Methods 0.000 claims description 35
- 238000010438 heat treatment Methods 0.000 claims description 6
- 238000012360 testing method Methods 0.000 claims description 5
- 230000002093 peripheral effect Effects 0.000 claims description 3
- 238000010008 shearing Methods 0.000 claims description 3
- 238000003745 diagnosis Methods 0.000 abstract description 2
- 230000008439 repair process Effects 0.000 abstract description 2
- 238000001514 detection method Methods 0.000 description 8
- 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
Abstract
Invention describes a kind of method detecting active sulfur content in insulating oil to comprise the steps: (1), get transformer insulating oil sample used; (2), be coated on Quartz crystal resonant sheet; (3), input nitrogen; (4), record the frequency f of Quartz crystal resonant sheet
1; (5), temperature is controlled to keep 0.5 ~ 10h between 90 ~ 150 DEG C; (6), record the frequency f of Quartz crystal resonant sheet
2; (7), calculate the frequency change Δ f of Quartz crystal resonant sheet; (8), calculate the content of active sulfur in transformer insulating oil used.Use this method easily and accurately quantitatively can detect the content of active sulfur in transformer oil, 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 the constant temperature oven 1 with 1, the oscillator of the QCM (Quartz Crystal Microbalance) 1 of Quartz crystal resonant sheet and sensor stand, band frequency counter, transformer insulating oil sample used 0.05 ~ 5ml, band draft tube and escape pipe and well heater;
(2), by step (1) got insulating oil sample application on the Quartz crystal resonant sheet of step (1) got QCM (Quartz Crystal Microbalance), again by this QCM (Quartz Crystal Microbalance) feeding step (1) set constant temperature oven, and by wire, the described Quartz crystal resonant sheet being coated with transformer insulating oil sample used 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;
(3), open draft tube and escape pipe that (2) step inserts the constant temperature oven of Quartz crystal resonant sheet, in constant temperature oven, input nitrogen 20 ~ 60min with 0.1 ~ 1L input quantity per hour by draft tube wherein, then close described draft tube and escape pipe;
(4), the setting up procedure (1) set frequency f being with the oscillator recording step of frequency counter (2) to insert the Quartz crystal resonant sheet in described constant temperature oven
1, record described constant temperature the temperature inside the box;
(5), open the well heater of step (1) set constant temperature oven, described constant temperature the temperature inside the box is controlled between 90 ~ 150 DEG C, keeps this temperature 0.5 ~ 10h;
(6), close described well heater, when described constant temperature the temperature inside the box drops to step (4) recorded temperature value, the frequency f of Quartz crystal resonant sheet in record constant temperature oven
2;
(7), according to formula Δ f=f
1-f
2, in formula, Δ f is frequency change, f
1for heating the frequency of front Quartz crystal resonant sheet, f
2for heating the frequency of rear Quartz crystal resonant sheet, calculate described Quartz crystal resonant sheet before step (2) with step (6) after during this period of time in frequency change Δ f;
(8), 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 described Quartz crystal resonant sheet before step (2) with step (6) after during this period of time in mass change Δ m namely corrode the quality of sulfur product.The value of this mass change Δ of gained m, divided by the volume of step (1) got transformer insulating oil sample used, is the content of active sulfur in described transformer insulating oil used.
The invention has the beneficial effects as follows: use this method easily and accurately quantitatively can detect the content of 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 with the commercially available QCM type QCM (Quartz Crystal Microbalance) 1 of Quartz crystal resonant sheet and sensor stand, band frequency counter commercially available 1, TTL type oscillator, entrust the commercially available DZF type constant temperature oven 1 of 220kV transformer insulating oil used sample 0.05ml, band draft tube and escape pipe and well heater;
(2), by step (1) got insulating oil sample application on the Quartz crystal resonant sheet of step (1) got QCM (Quartz Crystal Microbalance), again by this QCM (Quartz Crystal Microbalance) feeding step (1) set constant temperature oven, and by wire, the described Quartz crystal resonant sheet being coated with transformer insulating oil sample used is connected with peripheral hardware electrochemical quartz crystal microbalance testing workstation;
(3), open draft tube and escape pipe that (2) step inserts the constant temperature oven of Quartz crystal resonant sheet, in constant temperature oven, input nitrogen 20min with 0.1L input quantity per hour by draft tube wherein, then close described draft tube and escape pipe;
(4), the setting up procedure (1) set frequency f being with the oscillator recording step of frequency counter (2) to insert the Quartz crystal resonant sheet in described constant temperature oven
1, record described constant temperature the temperature inside the box;
(5), open the well heater of step (1) set constant temperature oven, described constant temperature the temperature inside the box is controlled, at 90 DEG C, to keep this temperature 0.5h;
(6), close described well heater, when described constant temperature the temperature inside the box drops to step (4) recorded temperature value, the frequency f of Quartz crystal resonant sheet in record constant temperature oven
2;
(7), according to formula Δ f=f
1-f
2, in formula, Δ f is frequency change, f
1for heating the frequency of front Quartz crystal resonant sheet, f
2for heating the frequency of rear Quartz crystal resonant sheet, calculate described Quartz crystal resonant sheet before step (2) with step (6) after during this period of time in frequency change Δ f;
(8), 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 described Quartz crystal resonant sheet before step (2) with step (6) after during this period of time in mass change Δ m.The value of this mass change Δ of gained m, divided by the volume of step (1) got transformer insulating oil sample used, is the content of active sulfur in described transformer insulating oil used.
Embodiment 2:
(1), get with the commercially available QCM type QCM (Quartz Crystal Microbalance) 1 of Quartz crystal resonant sheet and sensor stand, band frequency counter commercially available 1, TTL type oscillator, entrust the DZF type constant temperature oven 1 of 110kV transformer insulating oil sample used 5ml, band draft tube and escape pipe and well heater;
Step is (2) with embodiment 1;
(3), open draft tube and escape pipe that (2) step inserts the constant temperature oven of Quartz crystal resonant sheet, in constant temperature oven, input nitrogen 60min with 1L input quantity per hour by draft tube wherein, then close described draft tube and escape pipe;
Step is (4) with embodiment 1;
(5), open the well heater of step (1) set constant temperature oven, described constant temperature the temperature inside the box is controlled, at 150 DEG C, to keep this temperature 10h;
Step (6) ~ (8) with embodiment 1.
Claims (1)
1. detect a method for active sulfur content in insulating oil, the method comprises the steps:
(1), get the constant temperature oven 1 with 1, the oscillator of the QCM (Quartz Crystal Microbalance) 1 of Quartz crystal resonant sheet and sensor stand, band frequency counter, transformer insulating oil sample used 0.05 ~ 5ml, band draft tube and escape pipe and well heater;
(2), by step (1) got insulating oil sample application on the Quartz crystal resonant sheet of step (1) got QCM (Quartz Crystal Microbalance), again by this QCM (Quartz Crystal Microbalance) feeding step (1) set constant temperature oven, and by wire, the described Quartz crystal resonant sheet being coated with transformer insulating oil sample used is connected with peripheral hardware electrochemical quartz crystal microbalance testing workstation;
(3), open draft tube and escape pipe that (2) step inserts the constant temperature oven of Quartz crystal resonant sheet, in constant temperature oven, input nitrogen 20 ~ 60min with 0.1 ~ 1L input quantity per hour by draft tube wherein, then close described draft tube and escape pipe;
(4), the setting up procedure (1) set frequency f being with the oscillator recording step of frequency counter (2) to insert the Quartz crystal resonant sheet in described constant temperature oven
1, record described constant temperature the temperature inside the box;
(5), open the well heater of step (1) set constant temperature oven, described constant temperature the temperature inside the box is controlled between 90 ~ 150 DEG C, keeps this temperature 0.5 ~ 10h;
(6), close described well heater, when described constant temperature the temperature inside the box drops to step (4) recorded temperature value, the frequency f of Quartz crystal resonant sheet in record constant temperature oven
2;
(7), according to formula Δ f=f
1-f
2, in formula, Δ f is frequency change, f
1for heating the frequency of front Quartz crystal resonant sheet, f
2for heating the frequency of rear Quartz crystal resonant sheet, calculate described Quartz crystal resonant sheet before step (2) with step (6) after during this period of time in frequency change Δ f;
(8), 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 described Quartz crystal resonant sheet before step (2) with step (6) after during this period of time in mass change Δ m, the value of this mass change Δ of gained m, divided by the volume of step (1) got transformer insulating oil sample used, is the content of active sulfur in described transformer insulating oil used.
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| CN201410172583.6A CN103954521B (en) | 2014-04-28 | 2014-04-28 | Detect the method for active sulfur content in insulating oil |
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|---|---|---|---|
| CN201410172583.6A CN103954521B (en) | 2014-04-28 | 2014-04-28 | Detect the method for active sulfur content in insulating oil |
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| CN103954521B true CN103954521B (en) | 2016-04-20 |
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| CN109060953B (en) * | 2018-07-25 | 2021-08-10 | 国网湖南省电力有限公司 | Electrified detection device and method for moisture content of electrical insulating oil |
| CN108982660B (en) * | 2018-07-25 | 2021-08-10 | 国网湖南省电力有限公司 | Transformer insulating oil moisture content online monitoring device and method |
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