CN102507715A - Method for detecting antioxidant of electric oil - Google Patents
Method for detecting antioxidant of electric oil Download PDFInfo
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- CN102507715A CN102507715A CN2011103582176A CN201110358217A CN102507715A CN 102507715 A CN102507715 A CN 102507715A CN 2011103582176 A CN2011103582176 A CN 2011103582176A CN 201110358217 A CN201110358217 A CN 201110358217A CN 102507715 A CN102507715 A CN 102507715A
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Abstract
The invention discloses a method for detecting antioxidant of electric oil, which is realized through the following steps: a proper amount of supporting electrolyte solution is added into the electric oil to prepare a current conductive solution system; the relationship between different concentration of antioxidant and the current peak value of electrochemical reaction can be established by adopting the conventional electrochemical detection method, so that the concentration of antioxidant in an oil sample can be calculated and obtained according to the current peak value of the electrochemical reaction for the to-be-detected oil sample. The method disclosed by the invention is simple, convenient and quick to operate, has high sensitivity, low detection lower limit, accurate and reliable detection result as well as excellent repeatability and reproducibility, and is applicable to oxidation stability detection for various electric oils, including insulating oil, lubricating oil and fire resistant oil, that are used in the electric power industry.
Description
Technical field
The invention belongs to electrochemical detection method, be specifically related to a kind of detection method of oil for electric power anti-oxidant.
Background technology
Oil for electric power requires to have reliable physics, chemical property, particularly good insulation performance performance, still; Oxidation in use all can take place in all oil products, and under high temperature action, this oxidizing process also can be accelerated; The acid product that oxidation generates might form sludge even produce deposition, the various aspects of performance of oil for electric power is descended, but also can stop up oil circuit; Cause major accident, so oxidation stability is the important service condition and the quality requirements of oil for electric power.In order to prolong the serviceable life of equipment, need add specific compound therein and give oil product good anti-oxidative stability.The adding of anti-oxidant can delay the oxidation rate of oil product significantly, prolongs the serviceable life of oil product greatly.
Detect anti-oxidant method commonly used and mainly contain AAS, liquid phase chromatography, infra-red sepectrometry, gas chromatography etc.State Standard of the People's Republic of China GB 7602 adopts spectrophotometry anti-oxidant T501 content, and sample pretreatment is complicated, and used instrument and medicine are more, and the probability that produces personal error in the measuring process is bigger.In using the liquid chromatography for measuring oil for electric power, during oxidation preventive content,, the separating power of chromatographic column is descended, cause the poor repeatability of detection because of the variation of sample component polarity.Infra-red sepectrometry, gas chromatography technology for detection are accurate, are widely used but expensive instrument and equipment has restricted it.Therefore, it is significant to set up a kind of new simple and easy to do detection method.
Summary of the invention
The purpose of this invention is to provide a kind of simple and efficient to handlely, it is low to detect lower limit, and testing result and has the detection method of the oil for electric power anti-oxidant of good GRR accurately and reliably.
Realize that the technical scheme that goal of the invention adopts is: the detection method of oil for electric power anti-oxidant; Adopt conventional electrochemical detection method and use external standard method; The supporting electrolyte that in standard oil sample that contains anti-oxidant and oil sample to be measured, adds equivalent; Make the typical curve of known antioxidants concentration and electrochemical reaction current peak value in the said standard oil sample, record oil sample kinetic current peak value to be measured after, calculate the oxidation preventive content of this oil sample to be measured again according to said typical curve.
Another kind of technical scheme of the present invention is: adopt conventional electrochemical detection method and use internal standard method; The supporting electrolyte that in standard oil sample that contains anti-oxidant and oil sample to be measured, adds equivalent gets standard oil sample mixed liquor and oil sample mixed liquor to be measured respectively; After recording the kinetic current peak value of oil sample mixed liquor to be measured earlier; The standard oil sample mixed liquor that adds equivalent that in oil sample mixed liquor to be measured, goes forward one by one again gets different samples to be tested; Measure the corresponding kinetic current peak value of each sample to be tested, calculate the oxidation preventive content of oil sample to be measured according to the kinetic current peak value of each sample to be tested that records.
The detection architecture of using electrochemical method to measure oxidation preventive content in the oil for electric power among the present invention is to cooperate the conduction system that forms with supporting electrolyte through oil for electric power; Wherein supporting electrolyte comprises acid, alkali, the salt of organic or inorganic; And the WS or the organic solution of the acid of organic or inorganic, alkali, salt, the concentration of supporting electrolyte in oil for electric power is 0.01%-99.99%.
Electrochemical detection method used in the present invention is conventional cyclic voltammetry, linear sweep method, pulse voltammetry etc., and the research electrode is gold electrode, platinum electrode, glass-carbon electrode in the electrochemical detection method, and the window of electro-chemical test is-5V-5V.
The anti-oxidant of oil for electric power comprises natural or the synthetic anti-oxidant, DBPC 2,6 ditertiary butyl p cresol (T501), 2 for example, 4-dimethyl-6 tert-butyl phenol, 2,6-di-tert-butylphenol etc.
The characteristics of the inventive method are through in oil for electric power, adding the solution system that an amount of supporting electrolyte solution is mixed with electric conductivity; Adopt conventional electrochemical detection method to set up the relation of different antioxidant concentrations and electrochemical reaction current peak value, thereby calculate the concentration of anti-oxidant in this oil sample according to the electrochemical reaction current peak value of oil sample to be measured.The inventive method is simple and efficient to handle; Highly sensitive, it is low to detect lower limit, and testing result accurately and reliably; And have good GRR, be applicable to the employed detection that comprises all kinds of oil for electric power oxidation stabilities abilities of insulating oil, lubricating oil, fire resistant oil of power industry.
The inventive method Applied Electrochemistry measuring technology is carried out assay determination to the antioxidant content in oil for electrical power equipment index; Be that a kind of strong of existing antioxidant content in oil for electrical power equipment measuring method standard replenished; And monitor quickly through electrochemical techniques, can early warning transformer operation troubles degree and safe operation risk trend.
Be further described below in conjunction with accompanying drawing and embodiment specific embodiments of the invention.
Description of drawings
Fig. 1 is the external standard method typical curve synoptic diagram of embodiment 1.
Fig. 2 is the internal standard method curve synoptic diagram of embodiment 2.
Fig. 3 is the external standard method typical curve synoptic diagram of embodiment 3.
Embodiment
Embodiment 1
Preparation anti-oxidant DBPC 2,6 ditertiary butyl p cresol (T501) content is respectively 0.1%, 0.2%; 0.3%; Each 50g of transformer oil standard oil sample of 0.4%, 0.5%, the NaOH ethanolic solution of employing 0.01% is as supporting electrolyte; 0.01% the NaOH ethanolic solution of getting each standard oil sample 1g and 1000g respectively mix standard oil sample mixed liquor; The concentration of NaOH is 0.01% in the standard oil sample mixed liquor, after ultrasonic concussion evenly, uses gold electrode as the research electrode in the three-electrode system; Set up the typical curve of different antioxidant concentrations and electrochemical reaction current peak value in each standard oil sample mixed solution with the cyclic voltammetry of initial voltage-0.8V, final voltage 1.8V, sweep velocity 0.01V/s, as shown in Figure 1; 0.01% the NaOH ethanolic solution that other gets 1g transformer oil sample to be measured and 1000g mix oil sample mixed liquor to be measured; The electrochemical reaction current peak value that records oil sample mixed liquor to be measured with the same electrical chemical method is y, calculates the concentration x=0.265% of anti-oxidant in this transformer oil sample to be measured again according to typical curve shown in Figure 1 and external standard method.
Embodiment 2
Preparation anti-oxidant 2; 4-dimethyl-6 tert-butyl phenol content is 0.1% lubricating oil standard oil sample 50g; By mass ratio 1:99 with mix as the glacial acetic acid of supporting electrolyte after standard oil sample mixed liquor is for use, the concentration of glacial acetic acid is 99% in the standard oil sample mixed liquor; Other get 1g lubricating oil sample to be measured mix with the glacial acetic acid of 99g oil sample mixed liquor to be measured; After ultrasonic concussion evenly; Use platinum electrode as the research electrode in the three-electrode system, the kinetic current peak value that records oil sample mixed liquor to be measured with the linear volt-ampere scanning method of initial voltage-0.5V, final voltage 2.0V, sweep velocity 0.05V/s is y; The middle standard oil sample mixed liquor for preparing before the 100g that adds toward this oil sample mixed liquor to be measured gets sample to be tested No. 1 again, and the kinetic current peak value of measuring No. 1 sample to be tested with the same electrical chemical method is y1; Add 100g standard oil sample mixed liquor once more and get sample to be tested No. 2; And after the kinetic current peak value of measuring No. 2 samples to be tested is y2; Make curve, as shown in Figure 2, the oxidation preventive content that calculates lubricating oil sample to be measured according to this curve and internal standard method again is x=0.270%.
Embodiment 3
Preparation anti-oxidant 2; 6-di-tert-butylphenol content is respectively 0.1%; 0.2%, 0.3%, 0.4%; Each 500g of fire resistant oil standard oil sample of 0.5%; Adopt 1-butyl-3-methylimidazole hexafluorophosphate ionic liquid at room temperature as supporting electrolyte, get respectively each standard oil sample 500g mix with 1-butyl-3-methylimidazole hexafluorophosphate ionic liquid at room temperature of 500g standard oil sample mixed liquor, the concentration of ionic liquid at room temperature is 50.0% in the standard oil sample mixed liquor; After the ultrasonic concussion evenly; Use glass-carbon electrode as the research electrode in the three-electrode system, set up the typical curve of different antioxidant concentrations and electrochemical reaction current peak value in each standard oil sample mixed solution with the pulse voltammetry of initial voltage-0.8V, final voltage 0.8V, voltage increment 0.001V, amplitude 0.01V, pulse width 0.01s, sampling width 0.01s, as shown in Figure 3; Other get 500g fire resistant oil sample to be measured mix with 1-butyl-3-methylimidazole hexafluorophosphate ionic liquid at room temperature of 500g oil sample mixed liquor to be measured; The kinetic current peak value that records oil sample mixed liquor to be measured with the same electrical chemical method is y, is x=0.339% according to the concentration that calculates anti-oxidant in this fire resistant oil standard oil sample according to typical curve shown in Figure 3 and external standard method more again.
Principle of the present invention is; Set up the linear relationship between the antioxidant concentration and electrochemical response in the oil sample of laboratory preparation through the electrochemical method of routine; Measure the electrochemical response of oil sample to be measured again, thereby derive the concentration of anti-oxidant in the oil sample to be measured.
Supporting electrolyte among the present invention comprises acid, alkali, the salt of organic or inorganic, and the WS or the organic solution of the acid of organic or inorganic, alkali, salt.Preferable supporting electrolyte comprises: the formic acid in the organic acid, acetic acid, dodecylbenzene sulfonic acid; Hydrochloric acid in the mineral acid, sulfuric acid, nitric acid; Sodium methoxide in the organic base, potassium tert-butoxide, phenyl lithium; Potassium hydroxide in the inorganic base, NaOH, ammoniacal liquor; 1-butyl in the organic salt-3-methylimidazole hexafluorophosphate ionic liquid at room temperature; Sodium chloride in the inorganic salts, glazier's salt.Organic solvent: methyl alcohol, ethanol, second cyanogen etc.
Claims (6)
1. the detection method of
a kind of oil for electric power anti-oxidant; It is characterized in that adopting conventional electrochemical detection method and use external standard method; The supporting electrolyte that in standard oil sample that contains anti-oxidant and oil sample to be measured, adds equivalent; Make the typical curve of known antioxidants concentration and electrochemical reaction current peak value in the said standard oil sample, record oil sample kinetic current peak value to be measured after, calculate the oxidation preventive content of this oil sample to be measured again according to said typical curve.
2. the detection method of
oil for electric power anti-oxidant according to claim 1; It is characterized in that said supporting electrolyte comprises acid, alkali, the salt of organic or inorganic; And the WS or the organic solution of the acid of organic or inorganic, alkali, salt, the concentration of supporting electrolyte in oil sample to be measured is 0.01%-99%.
3. the detection method of
oil for electric power anti-oxidant according to claim 1 and 2; It is characterized in that said electrochemical detection method is cyclic voltammetry, linear sweep method, pulse voltammetry; The research electrode is gold electrode, platinum electrode, glass-carbon electrode in the electrochemical detection method, and the window of electro-chemical test is-5V-5V.
4. the detection method of
a kind of oil for electric power anti-oxidant; It is characterized in that adopting conventional electrochemical detection method and use internal standard method; The supporting electrolyte that in standard oil sample that contains anti-oxidant and oil sample to be measured, adds equivalent gets standard oil sample mixed liquor and oil sample mixed liquor to be measured respectively; After recording the kinetic current peak value of oil sample mixed liquor to be measured earlier; The standard oil sample mixed liquor that adds equivalent that in oil sample mixed liquor to be measured, goes forward one by one again gets different samples to be tested, measures the corresponding kinetic current peak value of each sample to be tested, calculates the oxidation preventive content of oil sample to be measured according to the kinetic current peak value of each sample to be tested that records.
5. the detection method of
oil for electric power anti-oxidant according to claim 4; It is characterized in that said supporting electrolyte comprises acid, alkali, the salt of organic or inorganic; And the WS or the organic solution of the acid of organic or inorganic, alkali, salt, the concentration of supporting electrolyte in oil sample to be measured is 0.01%-99%.
6.
are according to the detection method of claim 4 or 5 described oil for electric power anti-oxidants; It is characterized in that said electrochemical detection method is cyclic voltammetry, linear sweep method, pulse voltammetry; The research electrode is gold electrode, platinum electrode, glass-carbon electrode in the electrochemical detection method, and the window of electro-chemical test is-5V-5V.
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Cited By (17)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103323515A (en) * | 2013-03-29 | 2013-09-25 | 宁波出入境检验检疫局检验检疫技术中心 | Method for detecting residual anti-oxidant content in industrial lubricating oil while in operation |
| CN103760214A (en) * | 2013-12-31 | 2014-04-30 | 长沙理工大学 | Method for detecting antioxidant content in transformer oil by square wave voltammetry |
| CN103760215A (en) * | 2013-12-31 | 2014-04-30 | 长沙理工大学 | Method for detecting antioxidant content in transformer oil by using Tafel plots |
| CN103808789A (en) * | 2014-02-18 | 2014-05-21 | 广西电网公司电力科学研究院 | Method for detecting antioxidant content of transformer oil by step wave voltammetry method |
| CN103940888A (en) * | 2014-02-18 | 2014-07-23 | 广西电网公司电力科学研究院 | Method used for detecting anti-oxidant content of transformer oil via linear sweep voltammetry |
| CN103940889A (en) * | 2014-02-18 | 2014-07-23 | 广西电网公司电力科学研究院 | Method used for detecting anti-oxidant content of transformer oil via differential normal pulse voltammetry |
| CN103954520A (en) * | 2014-04-28 | 2014-07-30 | 国家电网公司 | Method for testing content of corrosive sulphur in insulating oil |
| CN104237362A (en) * | 2014-09-24 | 2014-12-24 | 中国石油化工股份有限公司 | Electrolyte solution and application thereof |
| CN104597101A (en) * | 2015-01-05 | 2015-05-06 | 武汉材料保护研究所 | Method for measuring antioxidant content in lubricating oil by use of linear sweep voltammetry |
| CN104807902A (en) * | 2015-04-27 | 2015-07-29 | 广东电网有限责任公司电力科学研究院 | Detection method of dibenzyl disulfide and antioxidant in insulating oil |
| CN105486735A (en) * | 2016-01-19 | 2016-04-13 | 桂盟链条（太仓）有限公司 | Quality monitoring system for lubricating oil for chain machining |
| CN106104240A (en) * | 2014-03-18 | 2016-11-09 | 日立金属株式会社 | Conductive resin composition and pressure sensor |
| CN109521089A (en) * | 2018-12-30 | 2019-03-26 | 广东电网有限责任公司 | Oxidation preventive content measuring method and device in a kind of insulating oil |
| CN110441381A (en) * | 2019-09-12 | 2019-11-12 | 广州机械科学研究院有限公司 | The electrochemical detection method of oxidation preventive content in a kind of lubricant |
| CN110530959A (en) * | 2019-09-12 | 2019-12-03 | 广州机械科学研究院有限公司 | A kind of quantitative evaluation method for predicting lubricant life |
| CN111795997A (en) * | 2020-06-09 | 2020-10-20 | 国网山东省电力公司电力科学研究院 | Method and system for measuring residual content of antioxidant in insulating oil |
| WO2022074280A1 (en) * | 2020-10-09 | 2022-04-14 | Bioquochem, S.L. | Method for measuring oxidation parameters of an organic sample |
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Cited By (23)
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| CN103323515A (en) * | 2013-03-29 | 2013-09-25 | 宁波出入境检验检疫局检验检疫技术中心 | Method for detecting residual anti-oxidant content in industrial lubricating oil while in operation |
| CN103760214A (en) * | 2013-12-31 | 2014-04-30 | 长沙理工大学 | Method for detecting antioxidant content in transformer oil by square wave voltammetry |
| CN103760215A (en) * | 2013-12-31 | 2014-04-30 | 长沙理工大学 | Method for detecting antioxidant content in transformer oil by using Tafel plots |
| CN103760214B (en) * | 2013-12-31 | 2016-03-23 | 长沙理工大学 | Square wave voltammetry is utilized to detect the method for Antioxygen Content in Transformer Oil |
| CN103760215B (en) * | 2013-12-31 | 2016-03-23 | 长沙理工大学 | A kind of method utilizing Ta Feiertu to detect Antioxygen Content in Transformer Oil |
| CN103940889A (en) * | 2014-02-18 | 2014-07-23 | 广西电网公司电力科学研究院 | Method used for detecting anti-oxidant content of transformer oil via differential normal pulse voltammetry |
| CN103940889B (en) * | 2014-02-18 | 2016-05-25 | 广西电网公司电力科学研究院 | Utilize the conventional pulse voltammetry of difference to detect the method for Antioxygen Content in Transformer Oil |
| CN103808789A (en) * | 2014-02-18 | 2014-05-21 | 广西电网公司电力科学研究院 | Method for detecting antioxidant content of transformer oil by step wave voltammetry method |
| CN103940888A (en) * | 2014-02-18 | 2014-07-23 | 广西电网公司电力科学研究院 | Method used for detecting anti-oxidant content of transformer oil via linear sweep voltammetry |
| CN106104240A (en) * | 2014-03-18 | 2016-11-09 | 日立金属株式会社 | Conductive resin composition and pressure sensor |
| CN103954520A (en) * | 2014-04-28 | 2014-07-30 | 国家电网公司 | Method for testing content of corrosive sulphur in insulating oil |
| CN103954520B (en) * | 2014-04-28 | 2016-03-30 | 国家电网公司 | A kind of method detecting active sulfur content in insulating oil |
| CN104237362A (en) * | 2014-09-24 | 2014-12-24 | 中国石油化工股份有限公司 | Electrolyte solution and application thereof |
| CN104597101A (en) * | 2015-01-05 | 2015-05-06 | 武汉材料保护研究所 | Method for measuring antioxidant content in lubricating oil by use of linear sweep voltammetry |
| 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 |
| CN104807902A (en) * | 2015-04-27 | 2015-07-29 | 广东电网有限责任公司电力科学研究院 | Detection method of dibenzyl disulfide and antioxidant in insulating oil |
| CN105486735A (en) * | 2016-01-19 | 2016-04-13 | 桂盟链条（太仓）有限公司 | Quality monitoring system for lubricating oil for chain machining |
| TWI649548B (en) * | 2016-01-19 | 2019-02-01 | 岳盟企業股份有限公司 | Detection system and method for industrial oil products |
| CN109521089A (en) * | 2018-12-30 | 2019-03-26 | 广东电网有限责任公司 | Oxidation preventive content measuring method and device in a kind of insulating oil |
| CN110441381A (en) * | 2019-09-12 | 2019-11-12 | 广州机械科学研究院有限公司 | The electrochemical detection method of oxidation preventive content in a kind of lubricant |
| CN110530959A (en) * | 2019-09-12 | 2019-12-03 | 广州机械科学研究院有限公司 | A kind of quantitative evaluation method for predicting lubricant life |
| CN111795997A (en) * | 2020-06-09 | 2020-10-20 | 国网山东省电力公司电力科学研究院 | Method and system for measuring residual content of antioxidant in insulating oil |
| WO2022074280A1 (en) * | 2020-10-09 | 2022-04-14 | Bioquochem, S.L. | Method for measuring oxidation parameters of an organic sample |
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Application publication date: 20120620 |