CN104007192A - Determination method for metal deactivator, furfural and anti-oxidant in insulating oil - Google Patents
Determination method for metal deactivator, furfural and anti-oxidant in insulating oil Download PDFInfo
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Abstract
The invention discloses a determination method for a metal deactivator, furfural and an anti-oxidant in insulating oil. The determination method employs high performance liquid chromatography for determination and comprises the following steps: (1) preparation of a standard solution; (2) pretreatment of a sample; and (3) determination: a step of respectively sucking up a standard solution sample and a test sample solution, injecting the standard solution sample and the test sample solution into a high performance liquid chromatograph and carrying out determination, wherein chromatographic conditions are that octadecylsilane chemically bonded silica is used as a filler, detection wavelength is 260 to 280 nm, flow velocity is 0.8 to 1.2 ml/min, methanol-water is used as a mobile phase, gradient elution is carried out, the volume ratio of methanol to water in the mobile phase at a time period of 1 to 8 min is 40-60%: 60-40% and the volume ratio of methanol to water in the mobile phase at a time period of 9 to 18 min is 90-100%: 10-0%. The method provided by the invention realizes simultaneous detection of the contents of the three organic matters consisting of furfural, the anti-oxidant T501 and the metal deactivator in one-needle sample introduction, so a great amount of manpower and material resources are saved, detection efficiency is improved, and friendliness to the environment is realized.
Description
Technical field
The present invention relates to chemical analysis technology field, particularly relate to the assay method of metal passivator, furfural and antioxidant in a kind of insulating oil.
Background technology
In recent years, the transformer fault causing because of the active sulfur in insulating oil both at home and abroad takes place frequently, and the safe and stable operation of electrical network has been caused to significant damage.Active sulfur refer under certain condition can be directly and metal react and generate element sulphur or the heat-labile sulfide of metal sulfide, they have higher corrosion activity to metal, can cause the corrosion and damage of equipment and materials, as elemental sulfur, sulfuretted hydrogen, mercaptan and some organic molecule sulfide.Work about electric power person is devoted to research and solve the scheme of active sulfur problem always.Metal passivator reacts and is widely used because suppressing active sulfur and copper.Benzotriazole and its derivative is the common metal passivator of a class, and common mainly containing is following several, is shown below.
The passivator major part that at present both at home and abroad transformer adds is Irgamet39 (N-[2-(2-ethylhexyl)-aminomethyl]-methyl benzotriazazole), is the potpourri of two kinds of isomerss.The mechanism of action of metal passivator is mainly that the nitrogen-atoms on its molecule contains lone pair electrons and the outermost d track of metallic atom forms coordination bond; metal outermost orbit forms back coordination key by electrical feedback to nitrogen-atoms again; form the diaphragm of the similar polymkeric substance of one deck in metal surface, thereby prevention copper sheet and active sulfur react (reaction equation is as follows).The interpolation of metal passivator makes active sulfur problem obtain alleviation, but does not fundamentally eliminate or reduce the content of active sulfur.In transformer operational process, metal passivator can consume gradually, and therefore in insulating oil, metal passivation agent content must tracking and monitoring.
In insulating oil, common are the little molecule of machine and have three kinds: the furfural of Furfural Treating Process and the aging generation of solid insulating material, the benzotriazole metal passivator adding in order to suppress active sulfur and antioxidant T501 (2,6-toluene di-tert-butyl phenol).And in actual production, furfural content is the one monitoring to solid insulating material degree of aging; Metal passivator can consume gradually along with the growth of working time, thereby causes, to the inhibiting disappearance of active sulfur, device security being caused a hidden trouble; Oxidation preventive content reduction can cause the aging acceleration of oil product, therefore needs to detect the content of these three kinds of materials.At present, in detection insulating oil, the method for furfural content has liquid phase chromatography and spectrophotometric method; The current domestic standard that do not have of method that detects metal passivator in insulating oil, has liquid phase chromatography abroad; The method that detects T501 content in insulating oil has spectrophotometric method, liquid phase chromatography, vapor-phase chromatography and Fourier's infra-red sepectrometry.
Detection to common above three kinds of organic molecules in insulating oil is that a kind of method is measured a kind of organism substantially, therefore, if measure this three kinds of materials, current method can only be points for three times, go one by one test, this not only needs to expend a large amount of manpower and materials, and separates the liquid wastes that produce to the larger burden of environment generation.
In the time of the organic molecule detecting in transformer oil, owing to having adopted the mode of liquid-liquid extraction, therefore in insulating oil, various organic molecules are extracted and separate together, and then enter detection system, therefore can detection each other be produced and be disturbed.Therefore, wish to find a kind of detection method, can eliminate the phase mutual interference that these organic molecules detect, these three kinds of materials can be separated simultaneously again, realize by single injected sampling, measure this three kinds of organic content simultaneously, not only save a large amount of manpower and materials, and greatly improve detection efficiency, more meet the requirement of low-carbon environment-friendly.
Summary of the invention
Based on this, the object of this invention is to provide a kind of assay method that can simultaneously detect metal passivator in insulating oil, furfural and antioxidant.
Concrete technical scheme is as follows:
An assay method for metal passivator, furfural and antioxidant in insulating oil, adopts high-performance liquid chromatogram determination, comprises the steps:
(1) preparation standard solution
Precision takes the standard substance of metal passivator, adds the blank oil of transformer, prepares the metal passivator standard solution of desired concn;
Precision takes the standard substance of furfural, adds the blank oil of transformer, prepares the furfural standard solution of desired concn;
Precision takes the standard substance of antioxidant, adds the blank oil of transformer, prepares the antioxidant standard solution of desired concn;
(2) sample pre-treatments
Precision takes standard solution or insulating oil testing sample, adds methanol solvate, and vibration 5-15min, then leaves standstill and centrifugally get supernatant liquor until methyl alcohol separates completely with oil phase, filters, and obtains standard solution sample or need testing solution;
(3) measure
Chromatographic condition: taking octadecylsilane chemically bonded silica as filling agent, detection wavelength is 260-280nm, flow velocity is 0.8-1.2ml/min, using methanol-water as mobile phase, carries out the mobile phase volume of gradient elution: 1-8min than being 40-60% methyl alcohol: 60-40% water; The mobile phase volume of 9-18min is than being 90-100% methyl alcohol: 10%-0% water;
The accurate standard solution sample of drawing, injects high performance liquid chromatography, measures to obtain typical curve;
The accurate need testing solution of drawing, injects high performance liquid chromatography, measures, and to obtain final product.
Therein in an embodiment, described metal passivator be benzotriazole, 5-methyl benzotriazazole, Irgamet30 (N-[2-(2-ethylhexyl)-aminomethyl]-1,2,4-triazole) or Irgamet39 (N-[2-(2-ethylhexyl)-aminomethyl]-methyl benzotriazazole).
Therein in an embodiment, described metal passivator is Irgamet39 (N-[2-(2-ethylhexyl)-aminomethyl]-methyl benzotriazazole).
In an embodiment, described antioxidant is 2,6-toluene di-tert-butyl phenol therein.
In an embodiment, the filter core using in the filtration step of step (2) is 0.22 μ m therein.
In an embodiment, the condition of described gradient elution is therein: the mobile phase volume ratio of 1-8min is 50% methyl alcohol: 50% water; The mobile phase volume ratio of 9-18min is 100% methyl alcohol: 0% water.
Advantage of the present invention is as follows:
(1) the present invention, by a series of experimental study, has set up the method for metal passivation agent content in a kind of high performance liquid chromatography detection insulating oil, and in the method, optimal flow phase ratio is that methyl alcohol is 50%:50% than water.Measure metal passivator when simultaneously, when furfural and tri-kinds of materials of antioxidant T501, adopt gradient elution method, optimal flow phase volume ratio is that 1-8min methyl alcohol is 50%:50% than water, and 9-18min methyl alcohol is 100%:0 than water.
(2) the present invention has not only realized the quantitative detection of metal passivator in insulating oil, and has realized a pin sample introduction and detected furfural simultaneously, three kinds of organic content of antioxidant T501 and metal passivator.Both avoid the interference that in oil, common organic molecule detects metal passivator, saved again a large amount of manpower and materials, improved detection efficiency, environmentally friendly.
(3) the present invention provides reference and thinking for the efficient detection of organic molecule in insulating oil.Effective detection that single injected sampling is realized organic molecule in more insulating oils is the new method of insulating oil efficient detection development.
Brief description of the drawings
Fig. 1 is that mobile phase volume ratio is 50% methyl alcohol: the Irgamet39 chromatogram (AU: absorbance when 50% water; Min: minute);
Fig. 2 is the typical curve of Irgamet39;
Fig. 3 is furfural and Irgamet39 chromatogram;
Fig. 4 is the chromatogram of furfural, Irgamet39 and T501;
Fig. 5 is furfural typical curve (R2=0.999451);
Fig. 6 is antioxidant T501 typical curve (R2=0.9989).
Embodiment
Below in conjunction with the drawings and specific embodiments, the application is further elaborated.
1.1 instrument and equipment
High performance liquid chromatograph: waterse2695, waters company of the U.S. produces; SunFireTMC18 chromatography column; Chromatographic work station; Analytical balance, is accurate to 0.001g; Mechanical oscillation instrument; Hydro-extractor.
1.2 reagent
Methyl alcohol: chromatographically pure.Water: meet the requirement of one-level water in GB/T6682.Standard substance: Irgamet39: analyze pure; Furfural: analyze pure; Antioxidant (2,6-toluene di-tert-butyl phenol): analyze pure.The blank oil of #25 transformer oil.
1.3 process of the test
1.3.1 the preparation of standard solution
Take standard substance Irgamet390.020g, add the blank oil of 25# transformer to 20g, mix, be made into the stock solution that concentration is 1000mg/kg.With the blank oil dilution of 25# transformer stock solution, the metal passivator standard solution (as 5mg/kg, 50mg/kg, 100mg/kg, 300mg/kg, 500mg/kg) of preparing desired concn is kept in Brown Glass Brown glass bottles and jars only and seals and is stored in shady place.
1.3.2 sample-pretreating method
Take the oil sample of 20g with analytical balance in the test tube with grinding port plug, add the methanol solvate of 5mL, 10min that sample is vibrated on mechanical vibrator, sample is standing centrifugal, until methyl alcohol separates completely with oil phase.With the syringe extraction supernatant liquor 2mL of 5mL, stand-by after the filter element filtering with 0.22 μ m.
2.1 qualitative test
After chromatograph and detector are stable, solution stand-by after filtering are injected to instrument and carry out qualitative test, to determine the retention time of Irgamet39 standard substance.
Flow velocity is set as 1mL/min, and sampling volume is 1 μ L, and UV-detector detects wavelength 270nm.First mobile phase ratio is decided to be to first alcohol and water each 50%, the appearance time of Irgamet39 is at 5-6 minute, and when reducing methanol usage to 40% time, appearance time is at 8-10 minute, this ratio relative time in test process is long and need more mobile phase, therefore should not adopt this ratio.When increasing methanol usage to 60% time, appearance time is at 3-4 minute, for fear of detection system unstability of base line phenomenon at the beginning to the interference detecting, also this mobile phase ratio of recommendation not.Consider listed three kinds of mobile phase ratios in table 1, it is all 50% that optimal flow phase ratio is decided to be to first alcohol and water ratio, and chromatogram when wherein first alcohol and water ratio is all 50% is referring to Fig. 1.
Table 1 mobile phase ratio and appearance time
| Sequence number | Methyl alcohol % | Water % | Appearance time, min |
| 1 | 40 | 60 | 8-10 |
| 2 | 50 | 50 | 5-6 |
| 3 | 60 | 40 | 3-4 |
2.2 quantitative test
The standard solution preparing by 1.3.1 is analyzed according to the standard solution of the good variable concentrations of 1.3.2 step process, and recording responses value (peak area).Can obtain typical curve by five kinds of concentration standard materials measuring 5～500mg/kg, referring to table 2 and Fig. 2.
The standard substance response (peak area) of table 2 variable concentrations
| Sequence number | Concentration, mg/kg | Irgamet39 response (peak area) |
| 1 | 5 | 190606 |
| 2 | 50 | 1963204 |
| 3 | 100 | 3428333 |
| 4 | 300 | 9451046 |
| 5 | 500 | 14783159 |
| 6 | Linear coefficient | 0.9981 |
In order further to verify the accuracy of this method, according to the standard solution of three parts of concentration known of test procedure 1.3 process of the test preparations, be respectively sample 1, sample 2 and sample 3, concentration is respectively 30mg/kg, 150mg/kg, 200mg/kg, and testing result is as shown in table 3.In the time that sample concentration is 30mg/kg, five results of replicate determination are respectively 27.733mg/kg, 27.862mg/kg, 27.799mg/kg, 27.917mg/kg, 27.938mg/kg, mean value is 27.850mg/kg, and between mean value and compound concentration, relative deviation is 7.17%, and the recovery is 92.3%.Five results of sample 2 replicate determination are respectively 156.470mg/kg, 155.852mg/kg, 157.570mg/kg, 156.083mg/kg, 156.425mg/kg, mean value is 156.48mg/kg, between mean value and compound concentration, relative deviation is 4.3%, and the recovery is 95.7%.Five results of sample 3 replicate determination are respectively 201.054mg/kg, 200.586mg/kg, 200.540mg/kg, 201.563mg/kg, 200.483mg/kg, mean value is 200.85mg/kg, between mean value and compound concentration, relative deviation is 0.4%, and the recovery is 99.6%.By the mensuration of above three kinds of concentration samples, when sample concentration is less than 100mg/kg, the recovery is greater than 90%, and when sample concentration is greater than 100mg/kg, the recovery is greater than 95%, illustrates that this method has good accuracy.
The analysis of table 3 recovery
| Measure number of times | Sample 1 (mg/kg) | Sample 2 (mg/kg) | Sample 3 (mg/kg) |
| 1 | 27.733 | 156.470 | 201.054 |
| 2 | 27.862 | 155.852 | 200.586 |
| 3 | 27.799 | 157.570 | 200.540 |
| 4 | 27.917 | 156.083 | 201.563 |
| 5 | 27.938 | 156.425 | 200.483 |
| Mean value | 27.850 | 156.48 | 200.85 |
| Compound concentration | 30 | 150 | 200 |
| Relative deviation % | 7.17 | 4.3 | 0.4 |
| Recovery % | 92.3 | 95.7 | 99.6 |
In addition from the operating transformer of interpolation passivator, draw oil sample 5 parts, be labeled as sample 4 to sample 8.Carry out sample preparation sample introduction according to test procedure 1.3.2 part, each sample replicate determination five times, the standard deviation of five measurement results is all in 0.5, and detailed data is as shown in table 4, illustrates that this detection method has good repeatability.
Table 4 repeatability is analyzed
2.3 influence factor
In the time of the metal passivator detecting in transformer oil, owing to having adopted the mode of liquid-liquid extraction, therefore in insulating oil, other organic molecule can be extracted and separate together with metal passivator, and then enters detection system, therefore can the detection of metal passivator be produced and be disturbed.
In insulating oil, common are the little molecule of machine and have antioxidant T501 (2,6-toluene di-tert-butyl phenol), two kinds, the furfural of subtractive process and the aging generation of solid insulating material.And in actual production, often need to detect antioxidant, the content of these three kinds of materials of furfural and metal passivator.At present, in detection insulating oil, the method for T501 content has spectrophotometric method, liquid phase chromatography and Fourier's infra-red sepectrometry.The method that detects furfural content in insulating oil has liquid phase chromatography and spectrophotometric method.Detection to common above two kinds of organic molecules in insulating oil is that a kind of method is measured a kind of organism substantially, therefore, if measure this three kinds of materials, current method can only be by three kinds of methods, this not only needs to expend a large amount of manpower and materials, and separates the mobile phase liquid wastes that produce to the larger burden of environment generation.
Therefore, the present embodiment finds a kind of detection method, can eliminate the phase mutual interference that these organic molecules detect, these three kinds of materials can be separated simultaneously again, realize by single injected sampling, measure this three kinds of organic content simultaneously, not only save a large amount of manpower and materials, and greatly improve detection efficiency, more meet the requirement of low-carbon environment-friendly.
Under the optimal conditions of test metal passivator, flow velocity is 1mL/min, and sampling volume is 1 μ L, and UV-detector detects wavelength 270nm, and mobile phase ratio first alcohol and water is each 50%, test T501, the mixed solution of furfural and Irgamet39.Flow velocity is set as 1mL/min, and sampling volume is 1 μ L, and in the time that the ratio of mobile phase methanol and water is 50:50, furfural can well separate with Irgamet39, and appearance time is respectively 2.5-3.0min and 5.0-6.0min, as shown in Figure 3.Because the molecular polarity of T501 is less than the molecular polarity of furfural and Irgamet39, therefore, under this condition, even if extend to 20 minutes working time, T501 does not still go out peak.
Regulate mobile phase ratio by increasing methanol content, realized the detection of T501.But two kinds of materials of furfural and Irgamet39 can not effectively be separated under attempted mobile phase ratio because polarity is close, occur overlap of peaks part.The mobile phase methanol of attempting has 60:40 than the ratio of water, 70:30, and 80:20,90:10 and 100:0 all can not separate these three kinds of materials simultaneously effectively.
Under isocratic elution condition, can not effectively above three kinds of organism be separated, therefore attempt realizing by the method for gradient elution effective separation of these three kinds of materials.Flow velocity is set as 1mL/min, and the mobile phase ratio of 1-8min is 50:50, allows furfural effectively separate with Irgamet39, and from 9min, mobile phase uses 100% methyl alcohol, and result has realized effective separation of three kinds of materials.Furfural appearance time is 2.5-3.0min, and the appearance time of Irgamet39 is 5.0-6.0min, and the appearance time of T501 is 13.0-13.5min, as shown in table 4 and Fig. 4.
Table 4 mobile phase ratio and appearance time
2.4 according to the standard solution of process of the test 1.3 these three kinds of organic substances of preparation, formulates respectively typical curve, and oil sample is extracted to the system that enters of processing, and separates when detection can realize this three kinds of materials and detects according to the method for gradient elution in table 4:
The general <1mg/kg of furfural content in transformer oil, oxidation preventive content is in 0.3% left and right, namely 3000ppm, metal passivator, generally in 100mg/kg left and right, has therefore selected following concentration range to formulate typical curve.
2.4.1 the formulation of furfural typical curve:
Furfural is dissolved in blank oil, prepares respectively 0.1mg/kg, 0.5mg/kg and 1mg/kg
Carry out sample pre-treatments according to 1.3.2 step, under best instrument condition, analyze, obtain typical curve as shown in Figure 5:
2.4.2 the formulation of antioxidant T501 typical curve:
Antioxidant T501 is dissolved in blank oil, prepares respectively 1000mg/kg, 2000mg/kg, 3500mg/kg and 5000mg/kg.
Carry out sample pre-treatments according to 1.3.2 step, under best instrument condition, analyze, obtain typical curve as shown in Figure 6:
2.4.3 the preparation of two kinds of concentration known mixed solutions and testing result:
3 conclusions
(1) by a series of experimental study, set up the method for metal passivation agent content in a kind of high performance liquid chromatography detection insulating oil, in the method, optimal flow phase volume ratio is that methyl alcohol is 50%:50% than water.Measure metal passivator when simultaneously, when furfural and tri-kinds of materials of antioxidant T501, adopt gradient elution method, optimal flow phase volume ratio is that 1-8min methyl alcohol is 50%:50% than water, and 9-15min methyl alcohol is 100%:0 than water.
(2) this method has not only realized the quantitative detection of metal passivator in insulating oil, and has realized a pin sample introduction and detected furfural simultaneously, three kinds of organic content of antioxidant T501 and metal passivator.Both avoid the interference that in oil, common organic molecule detects metal passivator, saved again a large amount of manpower and materials, improved detection efficiency, environmentally friendly.
(3) this method provides reference and thinking for the efficient detection of organic molecule in insulating oil.Effective detection that single injected sampling is realized organic molecule in more insulating oils is the new method of insulating oil efficient detection development.
The above embodiment has only expressed several embodiment of the present invention, and it describes comparatively concrete and detailed, but can not therefore be interpreted as the restriction to the scope of the claims of the present invention.It should be pointed out that for the person of ordinary skill of the art, without departing from the inventive concept of the premise, can also make some distortion and improvement, these all belong to protection scope of the present invention.Therefore, the protection domain of patent of the present invention should be as the criterion with claims.
Claims (6)
1. an assay method for metal passivator, furfural and antioxidant in insulating oil, is characterized in that, adopts high-performance liquid chromatogram determination, comprises the steps:
(1) preparation standard solution
Precision takes the standard substance of metal passivator, adds the blank oil of transformer, prepares the metal passivator standard solution of desired concn;
Precision takes the standard substance of furfural, adds the blank oil of transformer, prepares the furfural standard solution of desired concn;
Precision takes the standard substance of antioxidant, adds the blank oil of transformer, prepares the antioxidant standard solution of desired concn;
(2) sample pre-treatments
Precision takes standard solution or insulating oil testing sample, adds methanol solvate, and then vibration leaves standstill and centrifugally get supernatant liquor until methyl alcohol separates completely with oil phase, filters, and obtains standard solution sample or need testing solution;
(3) measure
Chromatographic condition: taking octadecylsilane chemically bonded silica as filling agent, detection wavelength is 260-280nm, flow velocity is 0.8-1.2ml/min, using methanol-water as mobile phase, carries out the mobile phase volume of gradient elution: 1-8min than being 40-60% methyl alcohol: 60-40% water; The mobile phase volume of 9-18min is than being 90-100% methyl alcohol: 10%-0% water;
The accurate standard solution sample of drawing, injects high performance liquid chromatography, measures to obtain typical curve;
The accurate need testing solution of drawing, injects high performance liquid chromatography, measures, and to obtain final product.
2. assay method according to claim 1, it is characterized in that, described metal passivator is benzotriazole, 5-methyl benzotriazazole, N-[2-(2-ethylhexyl)-aminomethyl]-1,2,4-triazole or N-[2-(2-ethylhexyl)-aminomethyl]-methyl benzotriazazole.
3. assay method according to claim 2, is characterized in that, described metal passivator is N-[2-(2-ethylhexyl)-aminomethyl]-methyl benzotriazazole.
4. assay method according to claim 1, is characterized in that, described antioxidant is 2,6-toluene di-tert-butyl phenol.
5. assay method according to claim 1, is characterized in that, the filter core using in the filtration step of step (2) is 0.22 μ m.
6. according to the assay method described in claim 1-5 any one, it is characterized in that, the condition of described gradient elution is: the mobile phase volume ratio of 1-8min is 50% methyl alcohol: 50% water; The mobile phase volume ratio of 9-18min is 100% methyl alcohol: 0% water.
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| CN107367559A (en) * | 2017-07-19 | 2017-11-21 | 云南电网有限责任公司电力科学研究院 | The detection method of oxidation preventive content in a kind of insulating oil |
| CN107367559B (en) * | 2017-07-19 | 2019-10-01 | 云南电网有限责任公司电力科学研究院 | The detection method of oxidation preventive content in a kind of insulating oil |
| CN107796888A (en) * | 2017-10-02 | 2018-03-13 | 国网山西省电力公司电力科学研究院 | Can accurate test transformer insulating oil furfural content method and its device |
| CN107987917A (en) * | 2017-12-11 | 2018-05-04 | 国网福建省电力有限公司 | Sulfur corrosion means of defence in a kind of transformer oil |
| CN110057941A (en) * | 2019-05-15 | 2019-07-26 | 广西电网有限责任公司南宁供电局 | Detection method based on furfural content in live transformer insulation oil |
| CN114018887A (en) * | 2021-11-05 | 2022-02-08 | 国网安徽省电力有限公司电力科学研究院 | Method for rapidly detecting antioxidant content in transformer insulating oil |
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Address after: 510080 Dongfeng East Road, Dongfeng, Guangdong, Guangzhou, Zhejiang Province, No. 8 Patentee after: ELECTRIC POWER RESEARCH INSTITUTE, GUANGDONG POWER GRID CO., LTD. Address before: 510080 Dongfeng East Road, Dongfeng, Guangdong, Guangzhou, Zhejiang Province, No. 8 Patentee before: Electrical Power Research Institute of Guangdong Power Grid Corporation |