CN106770184A - The detection method of content of MEK is dissolved in a kind of transformer oil - Google Patents
The detection method of content of MEK is dissolved in a kind of transformer oil Download PDFInfo
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- CN106770184A CN106770184A CN201710224947.4A CN201710224947A CN106770184A CN 106770184 A CN106770184 A CN 106770184A CN 201710224947 A CN201710224947 A CN 201710224947A CN 106770184 A CN106770184 A CN 106770184A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/65—Raman scattering
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Abstract
A kind of detection method of content the present invention relates to dissolve MEK in transformer oil, methods described passes through the content of methyl ethyl ketone that the raman spectrum strength of MEK in the transformer oil sample that detection methyl alcohol is pre-processed is obtained in transformer oil sample, rapid and convenient, sample pretreatment are simple, the degree of accuracy and sensitivity are high, testing cost is cheap, it is easy to interior promotion and application on a large scale.
Description
Technical field
The present invention relates to T ＆ D Technology field, and in particular to dissolve the content detection side of MEK in a kind of transformer oil
Method.
Background technology
Power transformer undertakes the tasks such as voltage conversion, electric energy distribution in power system, is most important in power system
Hub device, its operational reliability is related to the safety and stablization of power system.Power transformer once operationally occurs
Failure, can not only cause power transformer to damage or even scrap, it is also possible to cause the generation of large area blackout, cause huge
Economic loss.Tested and analyzed to dissolving aging character thing in transformer oil, be the monitoring of power transformer built-in electrical insulation
One of effective ways, it can in time find the paper insulated early stage deterioration of transformer oil.At present, the most frequently used insulating paper heat ageing
Index is dissolving CO, CO in oil2And the content of furfural, but due to CO, CO2Deng the easy loss of gas and furfural easily by insulating paper
The reasons such as absorption, it is difficult to accurately measure its real content, influence is based on dissolving CO, CO in oil2And the content of furfural judges transformation
The accuracy of the degree of aging of device.
The content of the invention
It is an object of the invention to provide the detection method of content that MEK is dissolved in a kind of new transformer oil, methods described
Content is higher with transformer oil, the more preferable MEK of stability is aging character thing, and its content is detected using Raman spectroscopy,
Not only rapid and convenient, sample pretreatment are simple, and the degree of accuracy and sensitivity are high, and testing cost is cheap, are adapted to transformer oilpaper
The diagnostic analysis of insulation ag(e)ing.
To achieve the above object, the present invention provides herein below：
The detection method of content of MEK is dissolved in a kind of transformer oil, is comprised the following steps：
(1) standard oil sample pretreatment：By standard oil sample：Methyl alcohol volume ratio 8-12:1 ratio, takes standard oil sample and methyl alcohol
Mixing, takes methanol layer stand-by；
(2) model：The Raman spectrogram of methanol layer obtained in determination step (1), with MEK concentration as abscissa, first and second
Ketone relative intensity is ordinate, sets up the Quantitative Analysis Model of MEK；
(3) oil sample pretreatment to be measured：The method of same step (1) is pre-processed to oil sample to be measured, obtains methanol layer stand-by；
(4) oil sample content of methyl ethyl ketone to be measured is determined：The Raman spectrogram of determination step (3) gained methanol layer, according to step
(2) Quantitative Analysis Model obtains the content of methyl ethyl ketone of oil sample to be measured.
According to the detection method of content that MEK is dissolved in transformer oil of the present invention, the standard oil sample described in step (1)
Compound method be dissolved in transformer oil to weigh MEK, prepare a series of standard oil sample known to concentration.
According to the detection method of content that MEK is dissolved in transformer oil of the present invention, the standard oil sample described in step (1)
Concentration be 0-400mg/L, such as a series of concentration be 400mg/L, 200mg/L, 100mg/L, 50mg/L, 20mg/L and 0mg/L
Standard oil sample.
According in transformer oil of the present invention dissolve MEK detection method of content, standard oil sample described in step (1) with
And the oil sample to be measured and the volume ratio of methyl alcohol described in step (4) are 10:1.
According to the detection method of content that MEK is dissolved in transformer oil of the present invention, shake is mixed into described in step (1)
Swing mixing or magnetic agitation mixing；Preferably, described mixing is magnetic agitation mixing.
According to the detection method of content that MEK is dissolved in transformer oil of the present invention, the MEK phase described in step (2)
Computational methods to intensity are, fixed to select a MEK raman spectra and a methyl alcohol raman spectra, MEK Raman spectrum
Peak-to-peak area is MEK relative intensity with the ratio of methyl alcohol raman spectra peak area；Preferably, MEK relative intensity is
The ratio of MEK characteristic peak peak area and methyl alcohol internal standard peak-to-peak area, wherein, described MEK characteristic peak and methyl alcohol internal standard
The selection principle at peak is in the detection range of Raman spectrometer, relative to neighbouring raman spectra, there is intensity higher and relative
It is independent, small raman spectra is influenceed by other raman spectras, MEK characteristic peak is 763cm as mentioned-1The raman spectra at place,
Described methyl alcohol internal standard peak is preferably 1450cm-1The raman spectra at place.
According to the detection method of content that MEK is dissolved in transformer oil of the present invention, the quantitative analysis described in step (2)
Model application least square method is set up.
According to the detection method of content that MEK is dissolved in transformer oil of the present invention, Raman Spectra described in step (2)
The condition determination of figure is 532nm wavelength lasers, laser power is 100mW, the time of integration is 3s, integral number of times is that 50, slit is wide
Spend for 50 μm, from 600l/500nm type gratings.
According to the detection method of content that MEK is dissolved in transformer oil of the present invention, the step (1), (2), (3) and (4)
Order can rationally exchange as needed, such as first determine the Raman spectrogram of the oil sample methanol layer to be measured of pretreatment, then determine
The standard oil sample Raman spectrogram of pretreatment, sets up Quantitative Analysis Model, and oil sample to be measured is obtained finally according to Quantitative Analysis Model
Content of methyl ethyl ketone.
The inventors discovered that, when the content detection of MEK is dissolved in using Raman spectroscopy to transformer oil, sample
Processing method it is larger on the influence of the accuracy and precision of testing result.Such as to the selection of oil sample reagent treatment, when selecting third
When ketone is processed oil sample, serious Raman signal interference is produced, directly affect the accuracy in detection of method；And be elected to and spend
When ionized water is processed oil sample, Raman signal intensity is weaker, influences the detection sensitivity of method；If from acetonitrile to oil
Sample is processed, and toxicity is big, and sensitivity is not also high.Selection methyl alcohol is processed oil sample, and oil sample presses 8-12 with methyl alcohol:1
Ratio mixing, the Raman spectrogram signal intensity of acquisition is strong, sensitivity can as little as 1.0mg/L, but if oil sample and methyl alcohol
Volume ratio is more than 12:1, methanol extraction efficiency is remarkably decreased, when oil sample and methyl alcohol volume ratio are 15:When 1, extraction efficiency only 60%
Left and right, has a strong impact on detection sensitivity, and works as oil sample and methyl alcohol volume ratio less than 8:When 1, content of methyl ethyl ketone is relatively low in methyl alcohol, also
The sensitivity of detection method can be influenceed.
The detection method of content of MEK is dissolved in the transformer oil that the present invention is provided, can be used in transformer oil dissolving
The quantification and qualification of MEK, simple to operate, safety, it is not necessary to which operating personnel have stronger specialty background, detection speed
Degree is fast, is that more accurately diagnosis oil paper insulation ageing state is laid a good foundation.
Brief description of the drawings
Fig. 1 is the Raman spectrogram that embodiment 1 determines MEK, methyl alcohol and extract；
Fig. 2 is the quantitative analysis figure that embodiment 3 is drawn.
Specific embodiment
Following examples are used to further describe the present invention, are not intended to limit the present invention.The instrument that is used in embodiment and
Reagent can be with commercially available.
The determination of the MEK characteristic peak of embodiment 1 and methyl alcohol internal standard peak
Weigh 400mg MEKs to be dissolved in 1L methyl alcohol, MEK extract is obtained.
From wavelength be 532nm, power for 100mW laser, (included using Confocal laser-scanning microscopy detection platform
Leica DM2700 types are just putting microscope, Andor SR-500i color dispersion-types Raman spectrometers and Andor iDus-416 types CCD
Etc. main devices) Raman spectrogram of pure MEK, pure methyl alcohol and MEK extract is determined, the time of integration is 3s, integration
Number is 100, slit width is 50 μm, grating is 600l/500nm type gratings, and detection range is 250-2500cm-1, as a result see figure
1, select 763cm-1The raman spectra at place is MEK characteristic peak, 1450-1The raman spectra at place is methyl alcohol internal standard peak.
The preparation of the standard oil sample of embodiment 2
400mg MEKs are weighed at room temperature in 1L transformer oil, it is the oil sample of 400mg/L that concentration is obtained, successively 2 times it is dilute
It is interpreted as the standard oil sample of one group of concentration respectively 200mg/L, 100mg/L and 50mg/L；Horn of plenty concentration gradient, and to 50mg/L
Standard oil sample is diluted the standard oil sample for obtaining 20mg/L.
The content of methyl ethyl ketone of embodiment 3 is determined
Step (1):Each concentration standard oil sample and 4mL methyl alcohol obtained in 40mL embodiments 2 are placed in 50mL tool plug palm fibres respectively
In color triangle flask, magnetic force constant temperature stirring 5min at 30 DEG C, just mixed liquor is poured into 50mL centrifuge tubes after being well mixed, with
The centrifugation 5min of 6000r/min, takes methanol layer stand-by；
Step (2)：The methyl alcohol that step (1) is obtained is placed in 751-10mm type quartz colorimetric utensils, from 532nm wavelength
Laser, laser power be 100mW, the time of integration be 3s, integral number of times be 50, slit width be 50 μm, from 600l/500nm
Type grating, the Raman spectroscopy of each concentration standard oil sample methanol layer obtained in determination step (1)；Using MATLAB softwares to drawing
After graceful spectrum spectrogram carries out the pretreatments such as miscellaneous peak removal, baseline adjustment and smoothing denoising, 763cm is chosen-1Locating raman spectra is
MEK characteristic peak, 1450cm-1Place's raman spectra is methyl alcohol internal standard peak, carries out intensity normalized, is corrected due to power waves
The peak intensity that dynamic, light path adjustment and focussing disparity cause fluctuates；Using calculating MEK feature peak-to-peak face in origin softwares
Product and its methyl alcohol internal standard peak-to-peak area, first is calculated according to formula (MEK Raman signatures peak area)/(methyl alcohol internal standard peak area)
Ethyl ketone, with respect to raman scattering intensity, is abscissa x with MEK concentration, and MEK relative intensity is ordinate y, as a result sees Fig. 2, is applied
Least square method sets up in oil the Quantitative Analysis Model for dissolving MEK, and obtaining MEK quantitative correction curve is：Y=1.28 ×
10-4x+8.96×10-6, its goodness of fit R2=0.9895.
Step (3)：Configuration MEK concentration is oil sample to be measured for the oil sample of 6.3mg/L, and the method for same step (1) is to be measured
Oil sample is pre-processed, and takes methanol layer stand-by；
Step (4):The Raman spectroscopy of oil sample methanol layer to be measured obtained in the method determination step (3) of same step (2),
MEK is with respect to raman scattering intensity at calculating, according to MEK quantitative correction curve y=1.28 × 10-4x+8.96×10-6Treated
The content of methyl ethyl ketone for surveying oil sample is 6.02mg/L.
With oil sample methanol layer to be measured obtained in step (3), as sample, repeat step (4) twice, obtains the first of oil sample to be measured
Ethyl ketone content is 5.75mg/L and 6.38mg/L, and the maximum deviation of detected value and actual value is no more than 8.73%, and the degree of accuracy is higher.
The content of methyl ethyl ketone of embodiment 4 is determined
Enchashment operating transformer paper oil insulation degradation failure oil sample is oil sample to be measured, is measured using headspace gas chromatography
Content of methyl ethyl ketone is 8.6mg/L in oil sample to be measured.
Step (1)：40mL oil samples to be measured and 4mL methyl alcohol are placed in 50mL tool plug brown conical flasks, magnetic force at 30 DEG C
Constant temperature stirs 5min, pours into 50mL centrifuge tubes mixed liquor after being well mixed, and with the centrifugation 5min of 6000r/min, takes
Methanol layer is stand-by；
Step (2)：The methyl alcohol that step (1) is obtained is placed in 751-10mm type quartz colorimetric utensils, from 532nm wavelength
Laser, laser power be 100mW, the time of integration be 3s, integral number of times be 50, slit width be 50 μm, from 600l/500nm
Type grating, the Raman spectroscopy of oil sample methanol layer to be measured obtained in determination step (1), according to the MEK that embodiment 3 is obtained
Quantitative correction curve y=1.28 × 10-4x+8.96×10-6The content of methyl ethyl ketone for obtaining oil sample to be measured is 9.56mg/L.
With oil sample methanol layer to be measured obtained in step (1), as sample, repeat step (2) twice, obtains the first of oil sample to be measured
Ethyl ketone content is 8.93mg/L and 7.93mg/L, and the maximum deviation of detected value and Headspace Gas Chromatography value is no more than
8.73%, the degree of accuracy is higher.
The content of methyl ethyl ketone assay method of embodiment 5 compares
Configuration MEK concentration is oil sample to be measured for the oil sample of 2.0mg/L.
Method 1：60mL oil samples to be measured and 4mL methyl alcohol are placed in 50mL tool plug brown conical flasks, magnetic force is permanent at 30 DEG C
Temperature stirring 5min, pours into 50mL centrifuge tubes mixed liquor after being well mixed, and with the centrifugation 5min of 6000r/min, takes first
Alcohol layer is stand-by；MEK contains in determining oil sample to be measured with the method (after divided by extraction proportionality coefficient 1.50) of the step of embodiment 4 (2)
It is 1.63mg/L to measure, and the maximum deviation of detected value and actual value is more than 18.50%, and measured value is relatively low；
Method 2：24mL oil samples to be measured and 4mL methyl alcohol are placed in 50mL tool plug brown conical flasks, magnetic force is permanent at 30 DEG C
Temperature stirring 5min, pours into 50mL centrifuge tubes mixed liquor after being well mixed, and with the centrifugation 5min of 6000r/min, takes first
Alcohol layer is stand-by；With content of methyl ethyl ketone in method (being multiplied by extraction proportionality coefficient 1.67) measure oil sample to be measured of the step of embodiment 4 (2)
It is 0mg/L, does not detect effective Raman signal of MEK, minimum detectable concentration is relatively low；
Method 3：40mL oil samples to be measured and 4mL methyl alcohol are placed in 50mL tool plug brown conical flasks, magnetic force is permanent at 30 DEG C
Temperature stirring 5min, pours into 50mL centrifuge tubes mixed liquor after being well mixed, and with the centrifugation 5min of 6000r/min, takes first
Alcohol layer is stand-by；It is 1.86mg/L to determine content of methyl ethyl ketone in oil sample to be measured with the method for the step of embodiment 4 (2), detected value and true
Real-valued maximum deviation is no more than 7.00%, and the degree of accuracy is higher；
Method 4：40mL oil samples to be measured and 4mL deionized waters are placed in 50mL tool plug brown conical flasks, magnetic at 30 DEG C
Power constant temperature stirs 5min, pours into 50mL centrifuge tubes mixed liquor after being well mixed, with the centrifugation 5min of 6000r/min,
Take layer of diw stand-by；The Raman spectroscopy of layer of diw is determined with the method for the step of embodiment 4 (2), is found without first
Ethyl ketone peak.
Claims (7)
1. the detection method of content of MEK is dissolved in a kind of transformer oil, is comprised the following steps：
(1) standard oil sample pretreatment：By standard oil sample：Methyl alcohol volume ratio 8-12:1 ratio, takes standard oil sample and methyl alcohol mixing,
Take methanol layer stand-by；
(2) model：The Raman spectrogram of methanol layer obtained in determination step (1), with MEK concentration as abscissa, MEK phase
It is ordinate to intensity, sets up the Quantitative Analysis Model of MEK；
(3) oil sample pretreatment to be measured：The method of same step (1) is pre-processed to oil sample to be measured, obtains methanol layer stand-by；
(4) oil sample content of methyl ethyl ketone to be measured is determined：The Raman spectrogram of determination step (3) gained methanol layer, according to step (2)
Quantitative Analysis Model obtains the content of methyl ethyl ketone of oil sample to be measured.
2. detection method of content according to claim 1, it is characterised in that：Standard oil sample described in step (1) and
The volume ratio of oil sample to be measured and methyl alcohol described in step (4) is 10:1.
3. detection method of content according to claim 1, it is characterised in that：The concussion that is mixed into described in step (1) is mixed
Close or magnetic agitation mixing；Preferably, it is described it is well mixed be magnetic agitation mixing.
4. detection method of content according to claim 1, it is characterised in that：MEK described in step (2) is relatively strong
The computational methods of degree are fixed selection one MEK raman spectra and a methyl alcohol raman spectra, MEK Raman spectrum peak-to-peak face
Product is MEK relative intensity with the ratio of methyl alcohol raman spectra peak area；Preferably, MEK relative intensity is MEK
The ratio of characteristic peak peak area and methyl alcohol internal standard peak-to-peak area.
5. detection method of content according to claim 1, it is characterised in that：Quantitative Analysis Model described in step (2)
Set up using least square method.
6. detection method of content according to claim 1, it is characterised in that：Raman spectroscopy described in step (2)
Condition determination is 532nm wavelength lasers, laser power is 100mW, the time of integration is 3s, integral number of times is that 50, slit width is
50 μm, from 600l/500nm type gratings.
7. the detection method of content described in any one of claim 1-6 transformer oil Aging of Oil-paper Insulation in Oil diagnosis in purposes.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107238596A (en) * | 2017-06-02 | 2017-10-10 | 重庆大学 | Method based on furfural in silver-based cavernous body substrate measuring transformer oil |
| CN109060768A (en) * | 2018-10-23 | 2018-12-21 | 江南大学 | A method of based on Surface enhanced Raman spectroscopy trace detection erythrosine concentration |
| CN110031443A (en) * | 2019-04-15 | 2019-07-19 | 重庆大学 | A kind of portable oil paper insulation ageing state Raman spectrum diagnostic device and method |
| CN110455776A (en) * | 2019-09-11 | 2019-11-15 | 重庆大学 | A method of detection furfural content in transformer oil |
| CN111551533A (en) * | 2020-05-11 | 2020-08-18 | 广东电网有限责任公司广州供电局 | Surface enhanced substrate, preparation method thereof and detection method of methanol in insulating oil |
| CN114813893A (en) * | 2021-01-18 | 2022-07-29 | 内蒙古电力(集团)有限责任公司内蒙古电力科学研究院分公司 | Detection box for detecting antioxidant content in transformer oil |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107238596A (en) * | 2017-06-02 | 2017-10-10 | 重庆大学 | Method based on furfural in silver-based cavernous body substrate measuring transformer oil |
| CN109060768A (en) * | 2018-10-23 | 2018-12-21 | 江南大学 | A method of based on Surface enhanced Raman spectroscopy trace detection erythrosine concentration |
| CN110031443A (en) * | 2019-04-15 | 2019-07-19 | 重庆大学 | A kind of portable oil paper insulation ageing state Raman spectrum diagnostic device and method |
| CN110455776A (en) * | 2019-09-11 | 2019-11-15 | 重庆大学 | A method of detection furfural content in transformer oil |
| CN111551533A (en) * | 2020-05-11 | 2020-08-18 | 广东电网有限责任公司广州供电局 | Surface enhanced substrate, preparation method thereof and detection method of methanol in insulating oil |
| CN114813893A (en) * | 2021-01-18 | 2022-07-29 | 内蒙古电力(集团)有限责任公司内蒙古电力科学研究院分公司 | Detection box for detecting antioxidant content in transformer oil |
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