CN104007192B - The assay method of metal passivator, furfural and antioxidant in insulating oil - Google Patents
The assay method of metal passivator, furfural and antioxidant in insulating oil Download PDFInfo
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Abstract
The invention discloses the assay method of metal passivator, furfural and antioxidant in a kind of insulating oil, adopt high-performance liquid chromatogram determination, comprise the steps: (1) preparation standard solution; (2) sample pre-treatments; (3) measure, chromatographic condition: take octadecylsilane chemically bonded silica as filling agent, determined wavelength is 260-280nm, and flow velocity is 0.8-1.2ml/min, using methanol-water as mobile phase, carry out gradient elution: the mobile phase volume of 1-8min is 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; Accurate absorption standard solution sample and need testing solution, inject high performance liquid chromatography, measure and get final product respectively.Present invention achieves a pin sample introduction and detect furfural simultaneously, antioxidant T501 and metal passivator three kinds of organic content, save a large amount of manpower and materials, improve detection efficiency, environmentally friendly.
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 caused because of the active sulfur in insulating oil both at home and abroad takes place frequently, and causes significant damage to the safe and stable operation of electrical network.Active sulfur refer under certain condition can directly and metal to react the element sulphur or heat-labile sulfide that generate metal sulfide, they have higher corrosion activity to metal, the corrosion and damage of equipment and materials can be caused, as elemental sulfur, sulfuretted hydrogen, mercaptan and some organic molecule sulfide.Work about electric power person is devoted to the scheme researching and solving active sulfur problem always.Metal passivator reacts because suppressing active sulfur and copper and is widely used.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 transformer adds both at home and abroad is at present Irgamet39 (N-[2-(2-ethylhexyl)-aminomethyl]-methyl benzotriazazole), is the potpourri of two kinds of isomerss.The mechanism of action of the metal passivator nitrogen-atoms mainly on its molecule contains lone pair electrons and the outermost d track of metallic atom forms coordination bond; electrical feedback is formed back coordination key to nitrogen-atoms by metal outermost orbit again; form the diaphragm of the similar polymkeric substance of one deck in metal surface, thus stop copper sheet and active sulfur to 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.
Common are machine Small molecular in insulating oil and have three kinds: the furfural of Furfural Treating Process and the aging generation of solid insulating material, in order to the benzotriazole metal passivator that suppresses active sulfur to add and antioxidant T501 (2,6-toluene di-tert-butyl phenol).And in actual production, furfural content is monitored the one of solid insulating material degree of aging; Metal passivator can consume gradually along with the growth of working time, thus causes, to the inhibiting disappearance of active sulfur, causing a hidden trouble to device security; Oxidation preventive content reduction can cause the aging acceleration of oil product, therefore needs the content detecting these three kinds of materials.At present, the method detecting furfural content in insulating oil has liquid phase chromatography and spectrophotometric method; In detection insulating oil, the method for metal passivator is domestic does not at present have standard, has liquid phase chromatography abroad; The method detecting T501 content in insulating oil has spectrophotometric method, liquid phase chromatography, vapor-phase chromatography and FTIR spectrum method.
Substantially be that a kind of method measures a kind of organism to the detection of above three kinds of organic molecules common in insulating oil, therefore, if measure this three kinds of materials, current method can only be points for three times, go test one by one, this not only needs at substantial manpower and materials, and the liquid wastes being separated generation produce larger burden to environment.
When detecting the organic molecule in transformer oil, owing to have employed the mode of liquid-liquid extraction, therefore in insulating oil, various organic molecule is extracted together and separates, and then enters detection system, therefore can produce interference to detection each other.Therefore, wish to find a kind of detection method, the mutual interference that these organic molecules detect can be eliminated, 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 simultaneously can 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, vibration 5-15min, then leaves standstill and centrifugally gets supernatant liquor until methyl alcohol is separated completely with oil phase, filter, obtain standard solution sample or need testing solution;
(3) measure
Chromatographic condition: take octadecylsilane chemically bonded silica as filling agent, determined wavelength is 260-280nm, flow velocity is 0.8-1.2ml/min, using methanol-water as mobile phase, carries out gradient elution: the mobile phase volume of 1-8min is 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;
Accurate absorption standard solution sample, injects high performance liquid chromatography, measures to obtain typical curve;
Accurate absorption need testing solution, injects high performance liquid chromatography, measures, to obtain final product.
Wherein in an embodiment, described metal passivator is benzotriazole, 5-methyl benzotriazazole, Irgamet30 (N-[2-(2-ethylhexyl)-aminomethyl]-1,2,4-triazole) or Irgamet39 (N-[2-(2-ethylhexyl)-aminomethyl]-methyl benzotriazazole).
Wherein in an embodiment, described metal passivator is Irgamet39 (N-[2-(2-ethylhexyl)-aminomethyl]-methyl benzotriazazole).
Wherein in an embodiment, described antioxidant is 2,6-toluene di-tert-butyl phenol.
Wherein in an embodiment, the filter core used in the filtration step of step (2) is 0.22 μm.
Wherein in an embodiment, 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.
Advantage of the present invention is as follows:
(1) the present invention is by a series of experimental study, and establish a kind of method that high performance liquid chromatography detects metal passivation agent content in insulating oil, in the method, optimal flow Phase Proportion is methyl alcohol is 50%:50% than water.When Simultaneously test metal passivator, when furfural and antioxidant T501 tri-kinds of materials, adopt gradient elution method, optimal flow phase volume ratio is 1-8min methyl alcohol be 50%:50%, 9-18min methyl alcohol than water is 100%:0 than water.
(2) the present invention not only achieves the quantitative detection of metal passivator in insulating oil, and achieves a pin sample introduction and detect furfural, antioxidant T501 and metal passivator three kinds of organic content simultaneously.Both avoided the interference that in oil, common organic molecule detects metal passivator, and in turn saved a large amount of manpower and materials, improve detection efficiency, environmentally friendly.
(3) the present invention is that the efficient detection of organic molecule in insulating oil provides reference and thinking.Effective detection that single injected sampling realizes organic molecule in more insulating oils is the new method that insulating oil efficient detection develops.
Accompanying drawing explanation
Fig. 1 is mobile phase volume ratio is 50% methyl alcohol: the Irgamet39 chromatogram (AU: absorbance during 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: the requirement meeting 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 25# transformer blank oil dilution stock solution, the metal passivator standard solution (as 5mg/kg, 50mg/kg, 100mg/kg, 300mg/kg, 500mg/kg) preparing desired concn is kept in Brown Glass Brown glass bottles and jars only also to seal 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 of band grinding port plug, add the methanol solvate of 5mL, vibrate sample on mechanical vibrator 10min, left standstill by sample centrifugal, until methyl alcohol is separated completely with oil phase.Supernatant liquor 2mL is extracted, with stand-by after the filter element filtering of 0.22 μm with the syringe of 5mL.
2.1 qualitative test
After chromatograph and detector are stablized, carry out qualitative test, to determine the retention time of Irgamet39 standard substance by filtering rear stand-by solution injection instrument.
Flow rate set is 1mL/min, and sampling volume is 1 μ L, UV-detector determined wavelength 270nm.First mobile phase ratio is decided to be first alcohol and water each 50%, the appearance time of Irgamet39 at 5-6 minute, when reduce methanol usage to 40% time, appearance time is at 8-10 minute, this ratio relative time in test process is longer and need more mobile phase, therefore should not adopt this ratio.When increase methanol usage to 60% time, appearance time at 3-4 minute, in order to avoid detection system unstability of base line phenomenon is at the beginning to the interference detected, also not this mobile phase ratio of recommendation.Consider listed three kinds of mobile phase ratios in table 1, optimal flow Phase Proportion being decided to be first alcohol and water ratio is all 50%, and chromatogram when wherein first alcohol and water ratio is all 50% is see 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 of the standard solution prepared by 1.3.1 according to the good variable concentrations of 1.3.2 step process is analyzed, and recording responses value (peak area).Typical curve can be obtained, see table 2 and Fig. 2 by the five kinds of concentration standard materials measuring 5 ~ 500mg/kg.
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 to verify the accuracy of this method further, the standard solution of three parts of concentration known is prepared according to test procedure 1.3 process of the test, 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.When sample concentration is 30mg/kg, replicate determination five results 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%.Sample 2 replicate determination five results 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%.Sample 3 replicate determination five results 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
| Pendulous frequency | 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 adding passivator, draw oil sample 5 parts, be labeled as sample 4 to sample 8.Carry out sample preparation and sample introduction according to test procedure 1.3.2 part, each sample parallel measures five times, and the standard deviation of five measurement results is all within 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
When detecting the metal passivator in transformer oil, owing to have employed the mode of liquid-liquid extraction, therefore in insulating oil, other organic molecule can be extracted and separates with metal passivator together with, and then enters detection system, therefore can produce the detection of metal passivator and disturb.
Common are machine Small molecular in insulating oil 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 furfural and these three kinds of materials of metal passivator.At present, the method detecting T501 content in insulating oil has spectrophotometric method, liquid phase chromatography and FTIR spectrum method.The method detecting furfural content in insulating oil has liquid phase chromatography and spectrophotometric method.Substantially be that a kind of method measures a kind of organism to the detection of above two kinds of organic molecules common in insulating oil, therefore, if measure this three kinds of materials, current method can only be by three kinds of methods, this not only needs at substantial manpower and materials, and the mobile phase liquid wastes being separated generation produce larger burden to environment.
Therefore, the present embodiment finds a kind of detection method, the mutual interference that these organic molecules detect can be eliminated, 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, UV-detector determined wavelength 270nm, mobile phase ratio first alcohol and water each 50%, test T501, the mixed solution of furfural and Irgamet39.Flow rate set is 1mL/min, and sampling volume is 1 μ L, and when the ratio of mobile phase methanol and water is 50:50, furfural can well be separated with Irgamet39, and appearance time is respectively 2.5-3.0min and 5.0-6.0min, as shown in Figure 3.Molecular polarity due to T501 is less than the molecular polarity of furfural and Irgamet39, and therefore under this condition, even if extend to 20 minutes working time, T501 does not still go out peak.
Regulating mobile phase ratio by increasing methanol content, achieving the detection of T501.But furfural and Irgamet39 two kinds of materials can not effectively be separated under attempted mobile phase ratio because polarity is close, occur overlap of peaks part.The mobile phase methanol attempted has 60:40 than the ratio of water, 70:30,80:20,90:10 and 100:0, all these three kinds of materials can not be separated simultaneously effectively.
Effectively above three kinds of organism can not be separated under isocratic condition, therefore attempt the effective separation being realized these three kinds of materials by the method for gradient elution.Flow rate set is the mobile phase ratio of 1mL/min, 1-8min is 50:50, allows furfural effectively be separated with Irgamet39, and from 9min, mobile phase uses 100% methyl alcohol, and result achieves effective separation of three kinds of materials.The appearance time of furfural appearance time to be the appearance time of 2.5-3.0min, Irgamet39 be 5.0-6.0min, T501 is 13.0-13.5min, as shown in table 4 and Fig. 4.
Table 4 mobile phase ratio and appearance time
2.4 prepare the standard solution of these three kinds of organic substances according to process of the test 1.3, formulate typical curve respectively, carry out extraction process enter system to oil sample, are separated to detect can realize detecting while these three kinds of materials according to the method for gradient elution in table 4:
The general <1mg/kg of furfural content in transformer oil, oxidation preventive content is about 0.3%, and namely 3000ppm, metal passivator, generally at about 100mg/kg, therefore have selected following concentration range to formulate typical curve.
2.4.1 the formulation of furfural typical curve:
Furfural is dissolved in blank oil, prepares 0.1mg/kg respectively, 0.5mg/kg and 1mg/kg
Carry out sample pre-treatments according to 1.3.2 step, analyze under the instrument condition of the best, 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 1000mg/kg respectively, 2000mg/kg, 3500mg/kg and 5000mg/kg.
Carry out sample pre-treatments according to 1.3.2 step, analyze under the instrument condition of the best, 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, establish a kind of method that high performance liquid chromatography detects metal passivation agent content in insulating oil, in the method, optimal flow phase volume ratio is methyl alcohol is 50%:50% than water.When Simultaneously test metal passivator, when furfural and antioxidant T501 tri-kinds of materials, adopt gradient elution method, optimal flow phase volume ratio is 1-8min methyl alcohol be 50%:50%, 9-15min methyl alcohol than water is 100%:0 than water.
(2) this method not only achieves the quantitative detection of metal passivator in insulating oil, and achieves a pin sample introduction and detect furfural, antioxidant T501 and metal passivator three kinds of organic content simultaneously.Both avoided the interference that in oil, common organic molecule detects metal passivator, and in turn saved a large amount of manpower and materials, improve detection efficiency, environmentally friendly.
(3) this method is that the efficient detection of organic molecule in insulating oil provides reference and thinking.Effective detection that single injected sampling realizes organic molecule in more insulating oils is the new method that insulating oil efficient detection develops.
The above embodiment only have expressed several embodiment of the present invention, and it describes comparatively concrete and detailed, but therefore can not 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 (3)
1. the assay method of 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; Described metal passivator is benzotriazole, 5-methyl benzotriazazole, N-[2-(2-ethylhexyl)-aminomethyl]-1,2,4-triazoles or N-[2-(2-ethylhexyl)-aminomethyl]-methyl benzotriazazole;
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; Described antioxidant is 2,6-toluene di-tert-butyl phenol;
(2) sample pre-treatments
Precision takes standard solution or insulating oil testing sample, adds methanol solvate, vibration, then leaves standstill and centrifugally gets supernatant liquor until methyl alcohol is separated completely with oil phase, filter, obtain standard solution sample or need testing solution;
(3) measure
Chromatographic condition: take octadecylsilane chemically bonded silica as filling agent, determined wavelength is 260-280nm, and flow velocity is 0.8-1.2ml/min, using methanol-water as mobile phase, carries out gradient elution: 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;
Accurate absorption standard solution sample, injects high performance liquid chromatography, measures to obtain typical curve;
Accurate absorption need testing solution, injects high performance liquid chromatography, measures, to obtain final product.
2. assay method according to claim 1, is characterized in that, described metal passivator is N-[2-(2-ethylhexyl)-aminomethyl]-methyl benzotriazazole.
3. assay method according to claim 1, is characterized in that, the filter core used in the filtration step of step (2) is 0.22 μm.
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| CN106370613B (en) * | 2016-11-10 | 2024-01-19 | 广东电网有限责任公司电力科学研究院 | Spectrum system and method for directly measuring concentration of furfural in transformer 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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