CN107796885A - Furans series derivates assay method in FR3 vegetable insulating oils - Google Patents
Furans series derivates assay method in FR3 vegetable insulating oils Download PDFInfo
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- CN107796885A CN107796885A CN201710822894.6A CN201710822894A CN107796885A CN 107796885 A CN107796885 A CN 107796885A CN 201710822894 A CN201710822894 A CN 201710822894A CN 107796885 A CN107796885 A CN 107796885A
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
Abstract
The present invention provides furans series derivates assay method in a kind of FR3 vegetable insulating oils, comprises the following steps：Instrument and equipment and reagent for liquid chromatographic detection is provided, liquid chromatographic detection condition is set；Methanol standard specimen and vegetable insulating oil oil ga(u)ge are prepared respectively；Qualitative analysis is carried out to each component using methanol standard specimen；Read each component appearance retention time and peak response peak height in methanol standard specimen；The vegetable insulating oil oil ga(u)ge of preparation is extracted, obtains oil ga(u)ge extract；Oil ga(u)ge extract, which is put into automatic sampler, carries out liquid-phase chromatographic analysis；Read each component appearance retention time and peak response peak height in oil ga(u)ge extract；The extraction yield of FR3 vegetable insulating oil oil ga(u)ges；Calculate furans series derivates each component concentration in FR3 vegetable insulating oils to be measured, the furans series derivates each component content dissolved in FR3 vegetable insulating oils can be accurately calculated by this method, so as to judge FR3 vegetable insulating oil transformer solid insulation states.
Description
Technical field
The present invention relates to a kind of liquid chromatogram measuring method of furans series derivates in FR3 vegetable insulating oils.
Background technology
The insulation system overwhelming majority of oil-filled transformer is paper oil insulation structure, mainly by liquid insulating medium (insulation
Oil) and solid dielectric insulation (oil-paper/oil immersion cardboard) collectively form.Because liquid insulating medium (insulating oil) is whole in transformer
It can be changed in individual operation lifecycle by the method for oil strain or replacing fresh oil, and solid dielectric insulation then almost can not be more
Change, therefore the service life of oil-filled transformer is mainly determined by solid dielectric insulation.How the solid of accurate judgement transformer
Dielectric state turns into the correct key for judging running state of transformer.
Insulating paper and cardboard in oil-filled electric equipment, its main component are cellulose, are normally transported in oil-filled electric equipment
The degraded or cracking of cellulosic material can all be caused when row and internal fault, corresponding catabolite is generated, such as carbohydrate and furan
Mutter derivative.Furans spreads out series derivates, can largely adsorb in the solid dielectric insulation of electrical equipment, small part is slightly soluble in
Oil, therefore, by detect the furan derivatives component that is slightly soluble in oil and content can determine whether oil-filled electric equipment running status and
Performance.On 12 international conference on large HV electric systems in 1984, British scholar proposes that furfural can be used as in operating transformer absolutely in oil first
The feature product of edge paper aging, the degradation of insulating materials can also be judged by detecting furfural content in insulating oil.Cellulose drops
Solution generates a part of D-Glucose monose.This D-Glucose monose is very unstable under the conditions of transformer station high-voltage side bus, is easily decomposed
A series of oxygenated heterocyclic compounds are generated, furfural is exactly one of which.Furfural is also referred to as furtural, and theory analysis and laboratory are ground
Study carefully oneself show, the generation of furfural in transformer oil, only from the degradation and decomposition of the insulation cellulosic material such as Paper or cardboard.
Therefore, furfural content changes in monitoring oil, it is possible to relatively accurately judges transformer solid insulation aging performance and development
Trend.
At present, the liquid insulating medium of oil-filled transformer is mainly mineral insulating oil, with green fluid insulation
The rise of medium vegetable insulating oil research, vegetable insulating oil is with its security performance high (burning-point >=300 DEG C), the good (biology of the feature of environmental protection
Degradation rate >=90%), wide material sources (oil crop seeds and plumule) the advantages that be increasingly becoming the good of mineral insulating oil and replaced
For product.According to incompletely statistics, existing 500,000 vegetable insulating oil transformer charging operations in the world, vegetable insulating oil transformer
Also the applicating history of 10 years has been had more than.The also progressively popularization and application of China's vegetable insulating oil transformer.
It is accurate to detect solid dielectric insulation deterioration/catabolite in vegetable insulating oil for vegetable insulating oil transformer
The content of (furans series derivates) in vegetable insulating oil turns into the correct pass for judging vegetable insulating oil running state of transformer
Key.Difference of the vegetable insulating oil with mineral insulating oil in molecule composition and chemical constitution, certainly will cause " vegetable insulating oil-paper "
System is with " mineral insulating oil-paper " system in solid dielectric insulation catabolite (furans series derivates) component and dissolving energy
Difference in power.At present, China is only detected to 2 furfural components in furans series derivates in mineral insulating oil, but is had
Research shows in " vegetable insulating oil-paper " system in solid dielectric insulation catabolite also to contain its in furans series derivates
Its component.China not yet proposes the analysis of furans series derivates and detection method in vegetable insulating oil at present.Therefore, establish and plant
Furans series derivatives thing liquid detection method is very necessary in thing insulating oil.
The content of the invention
The invention provides furans series derivates assay method in a kind of FR3 vegetable insulating oils, China is filled up and has planted
The blank of furans series derivates liquid chromatography detecting method in thing insulating oil.
Technical scheme：Furans series derivates assay method in a kind of FR3 vegetable insulating oils, including following step
Suddenly：
Step 1. provides the instrument and equipment and reagent for liquid chromatographic detection, sets liquid chromatographic detection condition；
It is 1.0mg/L's that step 2. prepares the furans series derivates methanol standard specimen that concentration is 1.0mg/L and concentration respectively
Furans series derivates FR3 vegetable insulating oil oil ga(u)ges；
Step 3. takes 1mL 1.0mg/L furans series derivates methanol standard specimens to be put into automatic sampler and carries out liquid chromatogram
Analysis, using 5 kinds of furans series derivates maximum absorption wavelengths in 1.0mg/L furans series derivates methanol standard specimens to each component
Carry out qualitative analysis；
Step 4. reads 5 kinds of furans series derivates each components in 1.0mg/L furans series derivates methanol standard specimens respectively
Appearance retention time and peak response peak height；
Step 5. extracts to the 1.0mg/L furans series derivates FR3 vegetable insulating oil oil ga(u)ges of preparation, obtains oil ga(u)ge
Extract；
Step 6. takes oil ga(u)ge extract resulting in 1mL steps 5 to be put into automatic sampler and carries out liquid-phase chromatographic analysis；
5 kinds of furans series derivates each component appearances retain in oil ga(u)ge extract obtained by step 7. read step 5
Time and peak response peak height；
5 kind furans series derivates each component appearance retention times of the step 8. according to detected by step 3 to step 7 and
Peak response peak height, calculate the extraction yield of 1.0mg/L furans series derivates FR3 vegetable insulating oil oil ga(u)ges；
Step 9. extracts according to step 5 to FR3 vegetable insulating oils to be measured, takes the extract to be measured obtained by 1mL to put
Enter and liquid-phase chromatographic analysis is carried out in automatic sampler, planted according to the 1.0mg/L furans series derivates FR3 obtained by step 8
The extraction yield of thing insulating oil oil ga(u)ge calculates furans series derivates each component concentration in FR3 vegetable insulating oils to be measured.
Instrument and equipment in the step 1 for liquid chromatographic detection includes high performance liquid chromatograph, and mechnical oscillator is high
Fast centrifuge, precision balance, tool fill in colorimetric cylinder with a scale.
The high performance liquid chromatograph includes
Pumping system：(or use) two kinds of solvents can at least be conveyed by possessing；
Sampling system：Automatic sampling apparatus or can accurate quantification to 10ul-20ul Manual quantitative devices；
Chromatographic column：The anti-phase post of carbon eight or carbon 18 post；
Detector：UV-detector, it is proposed that use diode array formula UV detectors；
Column oven：20 DEG C -65 DEG C of temperature control scope, temperature-controlled precision：±1℃；
Chromatographic work station：Collection, processing and parameter setting and the device failure alert function of data can be achieved；
On-line degassing device；
275 times/min ± 5 time of reciprocating vibration frequency/min of the mechnical oscillator, amplitude 35mm ± 3mm, temperature control model
Enclose：Room temperature -50, temperature-controlled precision：± 1 DEG C, the rotating speed 0r/min-4000r/min of the supercentrifuge, the precision balance
Precision is 0.1mg, and the capacity that the tool fills in colorimetric cylinder with a scale is 10mL.
It is for the reagent of liquid chromatographic detection in the step 1：
Methanol：High performance liquid chromatography is pure；
Water：Meet one-level water requirement in national standard GB/T 6682；
Furans series derivates：
HMF 5 hydroxymethyl 2 furaldehyde；
2- furfurals；
2- furfuryl alcohols；
2- acetyl furans；
5- methyl-2-furfurals；
Blank FR3 vegetable insulating oil oil samples：Its content is not more than 0.001mg/L in oil sample.
Setting liquid chromatographic detection condition is in the step 1：
Post case temperature：30℃；
Mobile phase volume ratio is：Methanol：Water=30%：70%；
Flow velocity：1.0mL/min；
Sample size：10ul；
Detection time：8min.
The method for the furans series derivates methanol standard specimen that preparation concentration is 1.0mg/L is in the step 2：Weigh respectively
Five kinds of HMF 5 hydroxymethyl 2 furaldehyde, 2- furfurals, 2- furfuryl alcohols, 2- acetyl furans, 5- methyl-2-furfurals each 0.020g of standard substance,
It is dissolved in 20mL methanol solutions, compound concentration 1000mg/L, takes 1000mg/L concentration standard liquids 1mL to move to 100mL appearances
It is 10mg/L with methanol dilution to the solution concentration in measuring bottle, absorption concentration is 10mg/L standard liquids 1.0mL to one groups of 10mL
In volumetric flask, diluted to obtain the standard liquid that concentration is 1.0mg/L with methanol solution, be placed on shady place and be kept in dark place.
The furans series derivates FR3 vegetable insulating oil oil calibration methods that concentration is 1.0mg/L in the step 2 are：Point
Also known as take five kinds of HMF 5 hydroxymethyl 2 furaldehyde, 2- furfurals, 2- furfuryl alcohols, 2- acetyl furans, 5- methyl-2-furfurals standard substances each
0.020g, it is dissolved in 20mL FR3 blank vegetable insulating oils, compound concentration 1000mg/L.Take 1000mg/L concentration standards molten
Liquid 1mL is moved in 100mL volumetric flasks, and it is 10mg/L to be diluted to the solution concentration with FR3 blank vegetable insulating oils, is drawn concentration and is
In 10mg/L standard liquids 10.0mL to one groups of 100mL volumetric flask, scale is diluted to FR3 blank vegetable insulating oils, with obtained
To the FR3 vegetable insulating oil standard liquids that concentration is 1.0mg/L, it is placed on shady place and is kept in dark place.
The side extracted in the step 5 to the 1.0mg/L furans series derivates FR3 vegetable insulating oil oil ga(u)ges of preparation
Extract is methanol in method, and specific method is：
FR3 vegetable insulating oils：Methanol=4mL:2mL；
Extract vibration temperature：30℃；
Extract duration of oscillation：20 minutes；
Extract centrifugation time：15 minutes；
Centrifuge speed：2000r/min.
The extraction yield of 1.0mg/L furans series derivates FR3 vegetable insulating oil oil ga(u)ges uses equation below in the step 8
Calculated：
Wherein：KiIn-extract, furans series derivates each component i extraction yields, %；
hIFR3 mark oil detection peak heightsIn -1.0mg/L furans series derivates FR3 vegetable insulating oil oil ga(u)ge methanol extraction liquid, each component
Detect peak height, mv；
hI methanol external standard detects peak heightIn -1.0mg/L furans series derivates methanol standard specimens, each component detection peak height, mv；
Voil- 1.0mg/L furans series derivates FR3 vegetable insulating oil oil ga(u)ge the volumes for extraction, mL；
VMethanol- methanol extraction liquid accumulates, mL.
Furans series derivates each component concentration is counted using below equation in FR3 vegetable insulating oils in the step 9
Calculate, it is desirable to which sample has same sampling volume with standard specimen.
Wherein：
Ci--- furans series derivates each component i concentration, mg/L in FR3 vegetable insulating oils
Ci,s--- the concentration of i components, mg/L in 1.0mg/L furans series derivates methanol standard specimens
Ai--- component i peak height, mv in extract to be measured
Ai,s--- 1.0mg/L furans series derivates methanol standard specimen components i peak height, mv
ki--- extraction yields of the component i under different extraction ratios, %.
The technique effect of the present invention：The furans series dissolved in FR3 vegetable insulating oils can be accurately calculated by this method to spread out
Biological each component content, so as to judge FR3 vegetable insulating oil transformer solid insulation states.
Brief description of the drawings
Fig. 1 is 5HMF, 2FAL, 2ACF and 2MEF typical case's chromatogram under Detection wavelength 276.8nm；
Fig. 2 is 2FOL and 2FAL typical case's chromatograms under Detection wavelength 216.5nm；
Fig. 3 is that 5HMF, 2FAL, 2ACF and 2MEF detect maximum absorption wavelength；
Fig. 4 is that 2FOL and 2FAL detects maximum absorption wavelength (under Detection wavelength 216.5nm)；
Embodiment
With reference to embodiment, the present invention is described in further detail, following examples be explanation of the invention and
The invention is not limited in following examples.
Furans series derivates in FR3 vegetable insulating oils, comprising HMF 5 hydroxymethyl 2 furaldehyde (5HMF), 2- furfuryl alcohols (2FAL),
5 kinds of 2- furfurals (2FOL), 2- acetyl furans (2ACF) and 5- methyl-2-furfurals (5MEF) materials, constitutive property are shown in Table 1.
The furans series derivates of table 1
Furans series derivates assay method uses liquid-liquid extraction method in FR3 vegetable insulating oils, by furans in insulating oil
Series derivates extract.Then extract is imported into high performance liquid chromatograph (HPLC) and analyzed.
The furans series derivatives analyte detection characteristic of table 2
| Component | 5HMF | 2FAL | 2FOL | 2ACF | 5MEF |
| Retention time (min) | 3.983 | 4.867 | 5.233 | 6.333 | 7.167 |
| Maximum absorption wavelength (nm) | 284.0 | 276.8 | 216.5 | 274.5 | 292.3 |
Furans series derivates assay method, comprises the following steps in a kind of FR3 vegetable insulating oils：
Step 1. provides the instrument and equipment and reagent for liquid chromatographic detection, sets liquid chromatographic detection condition；
It is 1.0mg/L's that step 2. prepares the furans series derivates methanol standard specimen that concentration is 1.0mg/L and concentration respectively
Furans series derivates FR3 vegetable insulating oil oil ga(u)ges；
Step 3. takes 1mL 1.0mg/L furans series derivates methanol standard specimens to be put into automatic sampler and carries out liquid chromatogram
Analysis, using 5 kinds of furans series derivates maximum absorption wavelengths in 1.0mg/L furans series derivates methanol standard specimens to each component
Carry out qualitative analysis；
Step 4. is respectively in 2- furfurals (2FAL) maximum absorption wavelength 276.8nm and 2- furfuryl alcohol (2FOL) maximum absorption wavelength
When 5 kinds of furans series derivates each component appearances reservations in 1.0mg/L furans series derivates methanol standard specimens are read under 216.5nm
Between and peak response peak height；
Step 5. extracts to the 1.0mg/L furans series derivates FR3 vegetable insulating oil oil ga(u)ges of preparation, obtains oil ga(u)ge
Extract；
Step 6. takes oil ga(u)ge extract resulting in 1mL steps 5 to be put into automatic sampler and carries out liquid-phase chromatographic analysis；
5 kinds of furans series derivates each component appearances retain in oil ga(u)ge extract obtained by step 7. read step 5
Time and peak response peak height；
5 kind furans series derivates each component appearance retention times of the step 8. according to detected by step 3 to step 7 and
Peak response peak height, calculate the extraction yield of 1.0mg/L furans series derivates FR3 vegetable insulating oil oil ga(u)ges；
Step 9. extracts according to step 5 to FR3 vegetable insulating oils to be measured, takes the extract to be measured obtained by 1mL to put
Enter and liquid-phase chromatographic analysis is carried out in automatic sampler, planted according to the 1.0mg/L furans series derivates FR3 obtained by step 8
The extraction yield of thing insulating oil oil ga(u)ge calculates furans series derivates each component concentration in FR3 vegetable insulating oils to be measured.
Instrument and equipment in the step 1 for liquid chromatographic detection includes high performance liquid chromatograph, and mechnical oscillator is high
Fast centrifuge, precision balance, tool fill in colorimetric cylinder with a scale.
The high performance liquid chromatograph includes
Pumping system：(or use) two kinds of solvents can at least be conveyed by possessing；
Sampling system：Automatic sampling apparatus or can accurate quantification to 10ul-20ul Manual quantitative devices；
Chromatographic column：The anti-phase post of carbon eight or carbon 18 post；
Detector：UV-detector, it is proposed that use diode array formula UV detectors；
Column oven：20 DEG C -65 DEG C of temperature control scope, temperature-controlled precision：±1℃；
Chromatographic work station：Collection, processing and parameter setting and the device failure alert function of data can be achieved；
On-line degassing device；
275 times/min ± 5 time of reciprocating vibration frequency/min of the mechnical oscillator, amplitude 35mm ± 3mm, temperature control model
Enclose：Room temperature -50, temperature-controlled precision：± 1 DEG C, the rotating speed 0r/min-4000r/min of the supercentrifuge, the precision balance
Precision is 0.1mg, and the capacity that the tool fills in colorimetric cylinder with a scale is 10mL.
It is for the reagent of liquid chromatographic detection in the step 1：
Methanol：High performance liquid chromatography is pure；
Water：Meet one-level water requirement in national standard GB/T 6682；
Furans series derivates：
HMF 5 hydroxymethyl 2 furaldehyde (5HMF)；
2- furfurals (2FAL)；
2- furfuryl alcohols (2FOL)；
2- acetyl furans (2ACF)；
5- methyl-2-furfurals (5MEF)；
Blank FR3 vegetable insulating oil oil samples：Its content is not more than 0.001mg/L in oil sample.
Setting liquid chromatographic detection condition is in the step 1：
Post case temperature：30℃；
Mobile phase volume ratio is：Methanol：Water=30%：70%；
Flow velocity：1.0mL/min；
Sample size：10ul；
Detection time：8min.
The method for the furans series derivates methanol standard specimen that preparation concentration is 1.0mg/L is in the step 2：Weigh respectively
Five kinds of HMF 5 hydroxymethyl 2 furaldehyde, 2- furfurals, 2- furfuryl alcohols, 2- acetyl furans, 5- methyl-2-furfurals each 0.020g of standard substance,
It is dissolved in 20mL methanol solutions, compound concentration 1000mg/L, takes 1000mg/L concentration standard liquids 1mL to move to 100mL appearances
It is 10mg/L with methanol dilution to the solution concentration in measuring bottle, absorption concentration is 10mg/L standard liquids 1.0mL to one groups of 10mL
In volumetric flask, diluted to obtain the standard liquid that concentration is 1.0mg/L with methanol solution, be placed on shady place and be kept in dark place.
The furans series derivates FR3 vegetable insulating oil oil calibration methods that concentration is 1.0mg/L in the step 2 are：Point
Also known as take five kinds of HMF 5 hydroxymethyl 2 furaldehyde, 2- furfurals, 2- furfuryl alcohols, 2- acetyl furans, 5- methyl-2-furfurals standard substances each
0.020g, it is dissolved in 20mL FR3 blank vegetable insulating oils, compound concentration 1000mg/L.Take 1000mg/L concentration standards molten
Liquid 1mL is moved in 100mL volumetric flasks, and it is 10mg/L to be diluted to the solution concentration with FR3 blank vegetable insulating oils, is drawn concentration and is
In 10mg/L standard liquids 10.0mL to one groups of 100mL volumetric flask, scale is diluted to FR3 blank vegetable insulating oils, with obtained
To the FR3 vegetable insulating oil standard liquids that concentration is 1.0mg/L, it is placed on shady place and is kept in dark place.
The side extracted in the step 5 to the 1.0mg/L furans series derivates FR3 vegetable insulating oil oil ga(u)ges of preparation
Extract is methanol in method, and specific method is：
FR3 vegetable insulating oils：Methanol=4mL:2mL；
Extract vibration temperature：30℃；
Extract duration of oscillation：20 minutes；
Extract centrifugation time：15 minutes；
Centrifuge speed：2000r/min.
The extraction yield of 1.0mg/L furans series derivates FR3 vegetable insulating oil oil ga(u)ges uses equation below in the step 8
Calculated：
Wherein：KiIn-extract, furans series derivates each component i extraction yields, %；
hIFR3 mark oil detection peak heightsIn -1.0mg/L furans series derivates FR3 vegetable insulating oil oil ga(u)ge methanol extraction liquid, each component
Detect peak height, mv；
hI methanol external standard detects peak heightIn -1.0mg/L furans series derivates methanol standard specimens, each component detection peak height, mv；
Voil- 1.0mg/L furans series derivates FR3 vegetable insulating oil oil ga(u)ge the volumes for extraction, mL；
VMethanol- methanol extraction liquid accumulates, mL.
The extraction yield of 1.0mg/L furans series derivates FR3 vegetable insulating oil oil ga(u)ges is calculated and posted such as table 3
The extraction yield of methanol extraction liquid in the 1.0mg/L furans series derivates FR3 vegetable insulating oil mark oil of table 3
Furans series derivates each component concentration is counted using below equation in FR3 vegetable insulating oils in the step 9
Calculate, it is desirable to which sample has identical sampling volume with standard specimen.
Wherein：
Ci--- furans series derivates each component i concentration, mg/L in FR3 vegetable insulating oils
Ci,s--- the concentration of i components, mg/L in 1.0mg/L furans series derivates methanol standard specimens
Ai--- component i peak height, mv in extract to be measured
Ai,s--- 1.0mg/L furans series derivates methanol standard specimen components i peak height, mv
ki--- extraction yields of the component i under different extraction ratios, %.
Each component content quantitative computational methods use external standard in furans series derivates assay method in FR3 vegetable insulating oils
Method, i.e., first prepare containing tested component concentration known C (Xi) standard specimen, using tested component concentration known standard specimen on chromatograph
Corresponding response peak height R (Xi) obtain the correction factor RF of the component(Xi)；It is unknown that the component is obtained under equal testing conditions again
Concentration samples corresponding response peak height A on chromatographi, utilize composition correction factor R F(Xi)It can be calculated by below equation
To the concentration of component C of the component unknown concentration samplei。
Component i concentration in sample：Ci=RF(Xi)× sample response value Ai
Correction factor RF(Xi)It is defined as：
Furans series derivates assay method in a kind of FR3 vegetable insulating oils of the present invention, mainly contains furans system
Prepared by row derivative methanol external standard and FR3 vegetable insulating oils mark oil, furans series derivates extraction side in FR3 vegetable insulating oils
Furans series derivates testing result in method, liquid-phase chromatographic analysis condition, extract sample analysis condition and FR3 vegetable insulating oils
Quantitative calculation method.The furans series derivates each component dissolved in FR3 vegetable insulating oils can be accurately calculated by this method to contain
Amount, so as to judge FR3 vegetable insulating oil transformer solid insulation states.
Claims (10)
1. furans series derivates assay method in a kind of FR3 vegetable insulating oils, it is characterised in that comprise the following steps：
Step 1. provides the instrument and equipment and reagent for liquid chromatographic detection, sets liquid chromatographic detection condition；
Step 2. prepares the furans series derivates methanol standard specimen that concentration is 1.0mg/L and the furans that concentration is 1.0mg/L respectively
Series derivates FR3 vegetable insulating oil oil ga(u)ges；
Step 3. takes 1mL 1.0mg/L furans series derivates methanol standard specimens to be put into automatic sampler and carries out liquid chromatogram point
Analysis, is entered using 5 kinds of furans series derivates maximum absorption wavelengths in 1.0mg/L furans series derivates methanol standard specimens to each component
Row qualitative analysis；
Step 4. reads 5 kinds of furans series derivates each component appearances in 1.0mg/L furans series derivates methanol standard specimens respectively
Retention time and peak response peak height；
Step 5. extracts to the 1.0mg/L furans series derivates FR3 vegetable insulating oil oil ga(u)ges of preparation, obtains oil ga(u)ge extraction
Liquid；
Step 6. takes oil ga(u)ge extract resulting in 1mL steps 5 to be put into automatic sampler and carries out liquid-phase chromatographic analysis；
5 kinds of furans series derivates each component appearance retention times in oil ga(u)ge extract obtained by step 7. read step 5
With peak response peak height；
5 kind furans series derivates each component appearance retention times and maximum of the step 8. according to detected by step 3 to step 7
Peak height is responded, calculates the extraction yield of 1.0mg/L furans series derivates FR3 vegetable insulating oil oil ga(u)ges；
Step 9. extracts according to step 5 to FR3 vegetable insulating oils to be measured, takes the extract to be measured obtained by 1mL to be put into certainly
Liquid-phase chromatographic analysis is carried out in dynamic injector, it is exhausted according to the 1.0mg/L furans series derivates FR3 plants obtained by step 8
The extraction yield of edge oil oil ga(u)ge calculates furans series derivates each component concentration in FR3 vegetable insulating oils to be measured.
2. furans series derivates assay method in a kind of FR3 vegetable insulating oils according to claim 1, its feature exist
In, the instrument and equipment in the step 1 for liquid chromatographic detection includes high performance liquid chromatograph, mechnical oscillator, at a high speed from
Scheming, precision balance, tool fill in colorimetric cylinder with a scale.
3. furans series derivates assay method in a kind of FR3 vegetable insulating oils according to claim 2, its feature exist
In the high performance liquid chromatograph includes
Pumping system：Possessing can at least convey or using two kinds of solvents；
Sampling system：Automatic sampling apparatus or can accurate quantification to 10ul-20ul Manual quantitative devices；
Chromatographic column：The anti-phase post of carbon eight or carbon 18 post；
Detector：UV-detector, it is proposed that use diode array formula UV detectors；
Column oven：20 DEG C -65 DEG C of temperature control scope, temperature-controlled precision：±1℃；
Chromatographic work station：Collection, processing and parameter setting and the device failure alert function of data can be achieved；
On-line degassing device；
275 times/min ± 5 time of reciprocating vibration frequency/min of the mechnical oscillator, amplitude 35mm ± 3mm, temperature control scope：Room
Temperature -50, temperature-controlled precision：± 1 DEG C, the rotating speed 0r/min-4000r/min of the supercentrifuge, the precision of the precision balance
For 0.1mg, the capacity that the tool fills in colorimetric cylinder with a scale is 10mL.
4. furans series derivates assay method in a kind of FR3 vegetable insulating oils according to claim 1, its feature exist
In the reagent in the step 1 for liquid chromatographic detection is：
Methanol：High performance liquid chromatography is pure；
Water：Meet one-level water requirement in national standard GB/T 6682；
Furans series derivates：
HMF 5 hydroxymethyl 2 furaldehyde；
2- furfurals；
2- furfuryl alcohols；
2- acetyl furans；
5- methyl-2-furfurals；
Blank FR3 vegetable insulating oil oil samples：Its content is not more than 0.001mg/L in oil sample.
5. furans series derivates assay method in a kind of FR3 vegetable insulating oils according to claim 1, its feature exist
In setting liquid chromatographic detection condition is in the step 1：
Post case temperature：30℃；
Mobile phase volume ratio is：Methanol：Water=30%：70%；
Flow velocity：1.0mL/min；
Sample size：10ul；
Detection time：8min.
6. furans series derivates assay method in a kind of FR3 vegetable insulating oils according to claim 1, its feature exist
In the method that the furans series derivates methanol standard specimen that concentration is 1.0mg/L is prepared in the step 2 is：5- hydroxyls are weighed respectively
Five kinds of methyl-2-furfural, 2- furfurals, 2- furfuryl alcohols, 2- acetyl furans, 5- methyl-2-furfurals each 0.020g of standard substance, dissolving
In 20mL methanol solutions, compound concentration 1000mg/L, 1000mg/L concentration standard liquids 1mL is taken to move to 100mL volumetric flasks
In, it is 10mg/L with methanol dilution to the solution concentration, absorption concentration is 10mg/L standard liquids 1.0mL to one groups of 10mL capacity
In bottle, diluted to obtain the standard liquid that concentration is 1.0mg/L with methanol solution, be placed on shady place and be kept in dark place.
7. furans series derivates assay method in a kind of FR3 vegetable insulating oils according to claim 1, its feature exist
In the furans series derivates FR3 vegetable insulating oil oil calibration methods that concentration is 1.0mg/L in the step 2 are：Weigh respectively
Five kinds of HMF 5 hydroxymethyl 2 furaldehyde, 2- furfurals, 2- furfuryl alcohols, 2- acetyl furans, 5- methyl-2-furfurals each 0.020g of standard substance,
It is dissolved in 20mL FR3 blank vegetable insulating oils, compound concentration 1000mg/L, takes 1000mg/L concentration standard liquids 1mL to move
Into 100mL volumetric flasks, it is 10mg/L to be diluted to the solution concentration with FR3 blank vegetable insulating oils, and absorption concentration is 10mg/L
In standard liquid 10.0mL to one groups of 100mL volumetric flask, scale is diluted to FR3 blank vegetable insulating oils, preparation obtains concentration
For 1.0mg/L FR3 vegetable insulating oil standard liquids, it is placed on shady place and is kept in dark place.
8. furans series derivates assay method in a kind of FR3 vegetable insulating oils according to claim 1, its feature exist
In in the method extracted in the step 5 to the 1.0mg/L furans series derivates FR3 vegetable insulating oil oil ga(u)ges of preparation
Extract is methanol, and specific method is：
FR3 vegetable insulating oils：Methanol=4mL:2mL；
Extract vibration temperature：30℃；
Extract duration of oscillation：20 minutes；
Extract centrifugation time：15 minutes；
Centrifuge speed：2000r/min.
9. furans series derivates assay method in a kind of FR3 vegetable insulating oils according to claim 8, its feature exist
In the extraction yield of 1.0mg/L furans series derivates FR3 vegetable insulating oil oil ga(u)ges is carried out using equation below in the step 8
Calculate：
Wherein：KiIn-extract, furans series derivates each component i extraction yields, %；
hIFR3 mark oil detection peak heightsIn -1.0mg/L furans series derivates FR3 vegetable insulating oil oil ga(u)ge methanol extraction liquid, each component detection
Peak height, mv；
hI methanol external standard detects peak heightIn -1.0mg/L furans series derivates methanol standard specimens, each component detection peak height, mv；
Voil- 1.0mg/L furans series derivates FR3 vegetable insulating oil oil ga(u)ge the volumes for extraction, mL；
VMethanol- methanol extraction liquid accumulates, mL.
10. furans series derivates assay method in a kind of FR3 vegetable insulating oils according to claim 9, its feature exist
In furans series derivates each component concentration is calculated using below equation in FR3 vegetable insulating oils in the step 9,
Ask sample and external standard that there is identical sampling volume.
<mrow>
<msub>
<mi>C</mi>
<mi>i</mi>
</msub>
<mo>=</mo>
<mfrac>
<msub>
<mi>A</mi>
<mi>i</mi>
</msub>
<msub>
<mi>A</mi>
<mrow>
<mi>i</mi>
<mo>,</mo>
<mi>s</mi>
</mrow>
</msub>
</mfrac>
<mo>&times;</mo>
<msub>
<mi>C</mi>
<mrow>
<mi>i</mi>
<mo>,</mo>
<mi>s</mi>
</mrow>
</msub>
<mo>&times;</mo>
<mfrac>
<mn>1</mn>
<msub>
<mi>k</mi>
<mi>i</mi>
</msub>
</mfrac>
<mo>-</mo>
<mo>-</mo>
<mo>-</mo>
<mrow>
<mo>(</mo>
<mn>2</mn>
<mo>)</mo>
</mrow>
</mrow>
Wherein：
Ci--- furans series derivates each component i concentration, mg/L in FR3 vegetable insulating oils
Ci,s--- the concentration of i components, mg/L in 1.0mg/L furans series derivates methanol standard specimens
Ai--- component i peak height, mv in extract to be measured
Ai,s--- 1.0mg/L furans series derivates methanol standard specimen components i peak height, mv
ki--- extraction yields of the component i under different extraction ratios, %.
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