CN106950216A - Content of acetone Raman spectra detection process is dissolved in transformer oil - Google Patents
Content of acetone Raman spectra detection process is dissolved in transformer oil Download PDFInfo
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- CN106950216A CN106950216A CN201710202138.3A CN201710202138A CN106950216A CN 106950216 A CN106950216 A CN 106950216A CN 201710202138 A CN201710202138 A CN 201710202138A CN 106950216 A CN106950216 A CN 106950216A
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- 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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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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Abstract
The invention discloses content of acetone Raman spectra detection process is dissolved in a kind of transformer oil, comprise the following steps：1) transformer oil sample is extracted：Acetone is extracted with methanol；2) Raman spectrum of extract is obtained：From 532nm wavelength incident laser light source to extract carry out Raman spectroscopy scans；3) Raman spectrogram is pre-processed：Miscellaneous peak removal, baseline adjustment and the pretreatment of smoothing denoising are carried out to extract Raman spectrogram, methanol 1034cm is chosen‑1It is that internal standard carries out intensity normalized to locate raman spectra；4) quantitative detection：Acetone characteristic peak and methanol internal standard peak area are calculated, and calculates acetone with respect to raman scattering intensity, according to acetone quantitative correction curve y=5.47 × 10 in transformer oil‑4x‑6.69×10‑4, x be acetone with respect to raman scattering intensity, y is acetone concentration.This method detection sensitivity is high, the degree of accuracy is high, test limit scope is wide.
Description
Technical field
The present invention relates to analysis detection field, and in particular to content of acetone Raman spectrum detection side is dissolved in transformer oil
Method.
Background technology
Large-scale power transformer plays act foot as the hub device of power system power system is defeated, during power transformation
The effect of weight, its safe operation is to ensureing that power system safety and stability is particularly important.It is exhausted by mineral insulating oil and fiber
The Oil-Paper Insulation of edge paper and cardboard composition is the main composition form of transformer interior insulation.In operating transformer ageing process
In, insulating oil and insulating paper can decompose and produce CO, CO in itself2, faults property and the insulation such as furfural and acetone
The material of performance, and be dissolved in oil.It is used as the property material for judging Transformer Insulation Aging index, CO, CO2And the component such as furfural
Assay method it is more ripe.But due to CO, CO2Reason is easily adsorbed etc. by insulating paper Deng the easy loss of gas and furfural,
Often it is difficult to accurately measure its real content, makes accurately to judge that the degree of aging of transformer is affected.
The features such as acetone has in oil steady dissolution, is difficult to adsorb, is difficult by environment temperature and air impact, by acetone
As the paper insulated aging characteristics of transformer oil, apply significant in the assessment of transformer oil Aging of Oil-paper Insulation in Oil.Mesh
Before, main application headspace gas chromatography detects the content of acetone in transformer oil both at home and abroad, but it has heating water bath operation
It is complicated, the problems such as go out sample equilibration time length, chromatographic column vulnerable to pollution and long detection time.In addition, headspace gas chromatography device
It is expensive, need periodic replacement part (such as chromatographic column) and safeguard to spend high, this causes the detection of headspace gas chromatography
Cost is higher.
In recent years, with the development of laser technology and charge coupled cell detection technique, Raman spectroscopy is extensive
In detection and performance evaluation applied to trace solid and fluent material.Raman spectroscopy uses laser as detection means,
Detection sample is not contacted, it is to avoid the destructivenesses of traditional chemical routes；Same sample can be carried out that detection is repeated several times, detection is steady
It is qualitative, reproducible；Equipment dependability is high, maintenance is small, and testing cost is relatively low.But operating transformer oil component is complicated, in addition
The content of acetone dissolved in transformer oil is relatively low, and Raman spectrum detection technique at this stage is not met by aging in transformer oil
The engineering actual demand of characteristic body content detection.
The content of the invention
Regarding the issue above, the present invention provides a kind of sensitivity is high, testing result accurately and reliably transformer
Content of acetone Raman spectra detection process is dissolved in oil.
The present invention solves the technical scheme that its technical problem is used：Content of acetone Raman spectrum is dissolved in a kind of transformer oil
Detection method, comprises the following steps：
1) transformer oil sample is extracted：The acetone in transformer oil sample to be measured is extracted with methanol, extracted
Take liquid；
2) Raman spectrum of extract is obtained：From 532nm wavelength incident laser light source to step 1) obtained extraction
Liquid carries out Raman spectroscopy scans, obtains the Raman spectrogram of extract；
3) Raman spectrogram is pre-processed：Miscellaneous peak removal, baseline adjustment are carried out to extract Raman spectrogram and is smoothly gone
Raman spectrogram at the pretreatment made an uproar, collection extract sample difference, chooses methanol 1034cm-1Place's raman spectra enters for internal standard
Row intensity normalized；
4) quantitative detection：Acetone characteristic peak and methanol internal standard peak area are calculated, and calculates acetone with respect to raman scattering intensity=the third
Ketone Raman signatures peak area/methanol internal standard peak area, according to acetone quantitative correction curve y=5.47 × 10 in transformer oil-4x-
6.69×10-4, the content of acetone dissolved in calculating transformer oil, x be acetone with respect to raman scattering intensity, y is acetone concentration.
In the above-mentioned technical solutions, by transformer oil sample to be measured and methanol according to volume ratio 10:1 is stirred mixing, so
After centrifuge, obtain upper strata extraction clear liquid.
In the above-mentioned technical solutions, the step 2) in extract carry out Raman spectroscopy scans when, the laser work(of selection
It 100mW, the time of integration is that 3s, integral number of times are that 50, slit width is 50 μm, from 600l/500nm type gratings that rate, which is,.
Preferably, the step 3) in the software that is pre-processed to extract Raman spectroscopy it is soft for MATLAB
Part.
Preferably, the step 4) middle Gauss peak type calculating acetone characteristic peak and methanol using in origin softwares
Internal standard peak area.
The beneficial effects of the invention are as follows：It can be used in transformer oil dissolving the quantification and qualification of acetone, operation letter
Single, safety, it is not necessary to which operating personnel have stronger specialty background, detection speed fast, are more accurately to diagnose paper oil insulation
Ageing state is laid a good foundation.The inventive method detection sensitivity is high, the degree of accuracy is high, test limit scope is wide.
Brief description of the drawings
Fig. 1 is pure acetone, pure methanol, the original Raman line of the methanol extraction liquid of acetone.
Fig. 2 is content of acetone correction graph in transformer oil.
Fig. 3 is the inventive method flow chart.
Embodiment
With reference to embodiment, the invention will be further described, but not thereby limiting the invention.
Embodiment 1 sets up in transformer oil the Quantitative Analysis Model for dissolving acetone
First, extractant is chosen
According to the similar principle that mixes, transformer is used as from methanol, acetonitrile, three deionized waters and dichloromethane successively
The extractant of acetone in oil.The effect of extracting of four kinds of extractants is contrasted, it is found that acetone Raman signal intensity is ordered as in extractant：
Methanol>Acetonitrile>Three deionized waters>Dichloromethane.In addition, acetonitrile belongs to medium poison class, toxicity is most strong；Three deionized waters
Density is more than transformer oil, it is necessary to carry out a point liquid using separatory funnel, increases the complexity of extraction procedure；Dichloromethane is to becoming
The extraction yield of acetone is very low in depressor oil, and can extract the fractions of transformer oil, can reduce the accuracy of detection.It is comprehensive
The factors such as toxicity, extraction process difficulty and extraction efficiency, final methanol of choosing is used as extractant.
2nd, pure acetone, pure methanol, the Raman spectrum of the methanol extraction liquid sample of acetone are determined
Pure acetone and the Raman spectrogram of pure methanol sample, optical maser wavelength are detected using Confocal laser-scanning microscopy detection platform
It 100mW, the time of integration is that 3s, integral number of times are that 100, slit width is 50 μm, from 600l/ to be from 532nm, laser power
500nm type gratings, gather the Raman spectrum of respective sample, and Raman spectrum detection range is 250-2500cm-1。
1) transformer oil sample is extracted
To reduce acetone volatilization and the influence of light, 40mL oil samples and 4mL methanol is taken to be placed in 50mL tool plug browns three respectively
In the flask of angle, and it is put into magnetic stir bar (30 DEG C) of constant temperature stirring 5min on magnetic stirring apparatus and makes it be sufficiently mixed；Will mixing
Liquid is poured into 50mL centrifuge tubes, is placed in supercentrifuge and is centrifuged 5min with 6000r/min, makes methanol extraction liquid and oil sample point
From, take upper strata extract clear liquid it is stand-by.
2) Raman spectrum of extract is obtained
By step 1) obtained extract is placed in 751-10mm type quartz colorimetric utensils；Quartz colorimetric utensil is placed in copolymerization burnt
On the objective table of Raman detection platform, the distance of adjustment microcobjective and sample focuses on laser spot in extract；From
It 100mW, the time of integration is that 3s, integral number of times are that 100, slit width is 50 μm, selection that 532nm wavelength lasers, laser power, which are,
600l/500nm type gratings, gather the Raman spectroscopy of extract.
3) Raman spectrum of methanol is pre-processed
For methanol solution feature, miscellaneous peak removal, baseline are carried out to extract Raman spectroscopy using MATLAB softwares
The pretreatment such as adjustment and smoothing denoising, to eliminate the interference such as cosmic ray, fluorescence background and noise of instrument；The same extraction of collection
The Raman spectrogram at liquid sample difference is taken, methanol 1034cm is chosen-1It is that internal standard carries out intensity normalized to locate raman spectra,
Correction is fluctuated due to peak intensity caused by power swing, light path adjustment and focussing disparity.
4) raman characteristic peak of the acetone in extract is chosen
Quantification and qualification for dissolving acetone in transformer oil, it is only necessary to choose single spectral peak and enter as feature spectral peak
Row quantitative analysis, selection principle is as follows：1. need to be in the detection range of Raman spectrometer；2. relative to neighbouring Raman spectrum
, there is higher intensity at peak；3. it is relatively independent, influenceed small by other raman spectras.The pure methanol of comparative analysis, pure acetone and acetone
The Raman spectral characteristics of methanol extraction liquid, as shown in figure 1, tentatively choosing 789cm-1It is used as acetone characteristic peak.Successively to difference third
The methanol solution of ketone content is detected, finds 789cm-1Place's acetone Raman signal reduces with the reduction of content of acetone, enters one
Step confirms 789cm-1For the Raman signal of acetone molecules.Finally select 789cm-1It is used as acetone characteristic peak.
3rd, set up in transformer oil and dissolve the Quantitative Analysis Model of acetone
Further to reduce influence of the testing conditions change to testing result, overlap of peaks, peak intensity and inspection are considered
Survey after the factors such as stability, choose methanol 1034cm-1Locate internal standard peak of the spectral peak as acetone；Different acetone concentrations are detected successively
In standard transformer oil sample, the standard transformer oil sample used content of acetone (mg/L) be followed successively by 6.4,13.1,23.6,48.7,
97.9th, 190.8, this 6 parts of samples are placed on the objective table of confocal detection platform and carry out Raman spectroscopy scans, phase is obtained
The original Raman line answered.Calculate the characteristic peak and its first of acetone in each sample respectively using the Gauss peak type in origin softwares
Alcohol internal standard peak area, and acetone is calculated with respect to raman scattering intensity (acetone Raman signatures peak area/methanol internal standard peak area)；With acetone
Relative raman scattering intensity be independent variable, oil in dissolving acetone content be dependent variable, using least square method set up oil in dissolve
The Quantitative Analysis Model of acetone, as shown in Fig. 2 obtaining acetone quantitative correction curve in transformer oil and being：Y=5.47 × 10-4x-
6.69×10-4, its goodness of fit R2=0.9934.
The transformer oil sample of the known acetone concentration of 2 pairs of preparations of embodiment carries out Raman spectrum detection
The standard transformer oil sample that content of acetone is 5.0mg/L has been prepared in laboratory, has been detected, in accordance with the following steps
Operate (operating process is as shown in Figure 3)：
1) transformer oil sample is extracted
Take 40mL standard transformers oil sample and 4mL methanol to be placed in 50mL tool plug brown conical flasks respectively, and be put into magnetic
Power stirrer (30 DEG C) another its of stirring 5min of constant temperature on magnetic stirring apparatus are sufficiently mixed；Then mixed liquor is poured into 50mL centrifugations
Guan Zhong, is placed in supercentrifuge and centrifuges 5min with 6000r/min, methanol extraction liquid is separated with oil sample, takes upper strata extraction clear
Liquid is stand-by.
2) Raman spectrum of extract is obtained
By step 1) in extract be placed in 751-10mm type quartz colorimetric utensils；Quartz colorimetric utensil is placed in copolymerization Jiao's drawing
On the objective table of graceful detection platform, the distance of adjustment microcobjective and sample focuses on laser spot in extract；From
It 100mW, the time of integration is that 3s, integral number of times are that 50, slit width is 50 μm, selection that 532nm wavelength lasers, laser power, which are,
600l/500nm type gratings, gather the Raman spectroscopy of extract.
3) Raman spectrum is pre-processed
Miscellaneous peak removal, baseline adjustment and smoothing denoising etc. are carried out to extract Raman spectrogram using MATLAB softwares pre-
Processing, to eliminate the interference such as cosmic ray, fluorescence background and noise of instrument；Gather the Raman spectrum at extract sample difference
Figure, chooses methanol 1034cm-1It is that internal standard carries out intensity normalized to locate raman spectra, and correction is adjusted due to power swing, light path
Peak intensity caused by whole and focussing disparity is fluctuated.
4) quantitatively detected according to the Quantitative Analysis Model built
The characteristic peak and its methanol internal standard peak area of acetone are calculated using the Gauss peak type in origin softwares, and calculates it
With respect to raman scattering intensity (acetone Raman signatures peak area/methanol internal standard peak area).According in the transformer oil obtained in embodiment 1
Acetone quantitative correction curve y=5.47 × 10-4x-6.69×10-4, calculate the content that acetone is dissolved in oil, three testing results
For：5.26mg/L, 5.13mg/L and 4.91mg/L.Content of acetone detected value is dissolved in oil and the maximum deviation of actual value is no more than
5.20%, the degree of accuracy is high.
Embodiment 3 is detected using Raman spectra detection process to the content of acetone in transformer oil sample
Enchashment operating transformer paper oil insulation degradation failure oil sample, its content of acetone is measured using headspace gas chromatography
For 6.8mg/L.Recycle the inventive method to carry out Raman spectrum detection to the sample, operate in accordance with the following steps：
1) transformer oil sample is extracted
Take 40mL oil samples and 4mL methanol to be placed in 50mL tool plug brown conical flasks respectively, and be put into magnetic stir bar and exist
(30 DEG C) stirring 5min of constant temperature make it be sufficiently mixed on magnetic stirring apparatus；Then mixed liquor is poured into 50mL centrifuge tubes, be placed in
5min is centrifuged with 6000r/min in supercentrifuge, methanol extraction liquid is separated with oil sample, takes upper strata to extract clear liquid stand-by.
2) Raman spectrum of extract is obtained
By step 1) in obtained extract be placed in 751-10mm type quartz colorimetric utensils；Quartz colorimetric utensil is placed in copolymerization
On the objective table of burnt Raman detection platform, the distance of adjustment microcobjective and sample focuses on laser spot in extract；Choosing
It 100mW, the time of integration is that 3s, integral number of times are that 50, slit width is 50 μm, selection to be with 532nm wavelength lasers, laser power
600l/500nm type gratings, gather the Raman spectroscopy of extract.
3) Raman spectrum is pre-processed
Miscellaneous peak removal, baseline adjustment and smoothing denoising etc. are carried out to extract Raman spectrogram using MATLAB softwares pre-
Processing, to eliminate the interference such as cosmic ray, fluorescence background and noise of instrument；Gather the Raman spectrum at extract sample difference
Figure, chooses methanol 1034cm-1It is that internal standard carries out intensity normalized to locate raman spectra, and correction is adjusted due to power swing, light path
Peak intensity caused by whole and focussing disparity is fluctuated.
4) quantitatively detected according to the Quantitative Analysis Model built
The characteristic peak and its methanol internal standard peak area of acetone are calculated using the Gauss peak type in origin softwares, and calculates it
With respect to raman scattering intensity (acetone Raman signatures peak area/methanol internal standard peak area).According in the transformer oil obtained in embodiment 1
Acetone quantitative correction curve y=5.47 × 10-4x-6.69×10-4, calculate the content that acetone is dissolved in oil, three testing results
For：6.38mg/L, 6.69mg/L and 6.49mg/L.Content of acetone detected value is dissolved in oil and the maximum deviation of actual value is no more than
6.17%, the degree of accuracy is high.
Claims (5)
1. content of acetone Raman spectra detection process is dissolved in a kind of transformer oil, it is characterised in that：Comprise the following steps：
1) transformer oil sample is extracted：The acetone in transformer oil sample to be measured is extracted with methanol, extract is obtained；
2) Raman spectrum of extract is obtained：From 532nm wavelength incident laser light source to step 1) obtained extract enters
Row Raman spectroscopy scans, obtain the Raman spectrogram of extract；
3) Raman spectrogram is pre-processed：Miscellaneous peak removal, baseline adjustment and smoothing denoising are carried out to extract Raman spectrogram
Raman spectrogram at pretreatment, collection extract sample difference, chooses methanol 1034cm-1It is that internal standard is carried out by force to locate raman spectra
Spend normalized；
4) quantitative detection：Acetone characteristic peak and methanol internal standard peak area are calculated, and calculates acetone and is drawn with respect to raman scattering intensity=acetone
Graceful characteristic peak area/methanol internal standard peak area, according to acetone quantitative correction curve y=5.47 × 10 in transformer oil-4x-6.69
×10-4, the content of acetone dissolved in calculating transformer oil, x be acetone with respect to raman scattering intensity, y is acetone concentration.
2. content of acetone Raman spectra detection process is dissolved in transformer oil as claimed in claim 1, it is characterised in that：It is described
Step 1) in extracting process be：By transformer oil sample to be measured and methanol according to volume ratio 10:1 is stirred mixing, Ran Houli
The heart, obtains upper strata extraction clear liquid.
3. content of acetone Raman spectra detection process is dissolved in transformer oil as claimed in claim 1, it is characterised in that：It is described
Step 2) in when carrying out Raman spectroscopy scans to extract, the laser power of selection be 100mW, the time of integration be 3s, integration
Number is that 50, slit width is 50 μm, from 600l/500nm type gratings.
4. content of acetone Raman spectra detection process is dissolved in transformer oil as claimed in claim 1, it is characterised in that：It is described
Step 3) in the software that is pre-processed to extract Raman spectroscopy be MATLAB softwares.
5. content of acetone Raman spectra detection process is dissolved in transformer oil as claimed in claim 1, it is characterised in that：It is described
Step 4) middle Gauss peak type calculating acetone characteristic peak and methanol internal standard peak area using in origin softwares.
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109030449A (en) * | 2018-04-25 | 2018-12-18 | 中国民航科学技术研究院 | A kind of lubricating oil and mixture ratio of fuel to oil rapid detection method |
| CN110874548A (en) * | 2018-08-31 | 2020-03-10 | 天津理工大学 | Lung cancer cell and normal cell recognition method based on combination of Raman spectrum and SVM |
| CN110879222A (en) * | 2019-11-06 | 2020-03-13 | 广州供电局有限公司 | Construction method of quantitative analysis curve of furfural in transformer oil and detection method of furfural content |
| CN111562247A (en) * | 2019-02-13 | 2020-08-21 | 中国石油天然气股份有限公司 | Hydrogen sulfide and carbon dioxide on-line analysis device and method |
| CN111562248A (en) * | 2020-05-15 | 2020-08-21 | 云南电网有限责任公司电力科学研究院 | Based on SF6Internal standard GIS fault diagnosis method |
| CN113533303A (en) * | 2021-08-19 | 2021-10-22 | 广西电网有限责任公司电力科学研究院 | Method for measuring content of benzotriazole in transformer oil |
| CN113624737A (en) * | 2021-07-05 | 2021-11-09 | 广东电网有限责任公司广州供电局 | Transformer oil extraction element and check out test set |
| CN113655050A (en) * | 2021-08-17 | 2021-11-16 | 南京富岛信息工程有限公司 | Method for improving Raman spectrum detection limit of trace crude oil in light oil |
| CN113686835A (en) * | 2021-10-11 | 2021-11-23 | 重庆大学 | Method for simultaneously detecting multiple characteristic substances in insulating oil based on liquid-liquid extraction and Raman spectroscopy |
| CN113985218A (en) * | 2021-09-20 | 2022-01-28 | 重庆大学 | Oil paper insulation aging diagnosis method based on fluorescent color |
| CN114113030A (en) * | 2021-10-14 | 2022-03-01 | 广东电网有限责任公司广州供电局 | Construction method of analysis model for acetone content in transformer oil and detection method for acetone content |
| 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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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109030449A (en) * | 2018-04-25 | 2018-12-18 | 中国民航科学技术研究院 | A kind of lubricating oil and mixture ratio of fuel to oil rapid detection method |
| CN110874548A (en) * | 2018-08-31 | 2020-03-10 | 天津理工大学 | Lung cancer cell and normal cell recognition method based on combination of Raman spectrum and SVM |
| CN111562247B (en) * | 2019-02-13 | 2023-06-30 | 中国石油天然气股份有限公司 | Hydrogen sulfide and carbon dioxide on-line analysis device and method |
| CN111562247A (en) * | 2019-02-13 | 2020-08-21 | 中国石油天然气股份有限公司 | Hydrogen sulfide and carbon dioxide on-line analysis device and method |
| CN110879222A (en) * | 2019-11-06 | 2020-03-13 | 广州供电局有限公司 | Construction method of quantitative analysis curve of furfural in transformer oil and detection method of furfural content |
| CN111562248A (en) * | 2020-05-15 | 2020-08-21 | 云南电网有限责任公司电力科学研究院 | Based on SF6Internal standard GIS fault diagnosis method |
| 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 |
| CN113624737A (en) * | 2021-07-05 | 2021-11-09 | 广东电网有限责任公司广州供电局 | Transformer oil extraction element and check out test set |
| CN113655050A (en) * | 2021-08-17 | 2021-11-16 | 南京富岛信息工程有限公司 | Method for improving Raman spectrum detection limit of trace crude oil in light oil |
| CN113655050B (en) * | 2021-08-17 | 2024-04-26 | 南京富岛信息工程有限公司 | Method for improving Raman spectrum detection limit of trace crude oil in light oil |
| CN113533303A (en) * | 2021-08-19 | 2021-10-22 | 广西电网有限责任公司电力科学研究院 | Method for measuring content of benzotriazole in transformer oil |
| CN113985218A (en) * | 2021-09-20 | 2022-01-28 | 重庆大学 | Oil paper insulation aging diagnosis method based on fluorescent color |
| CN113985218B (en) * | 2021-09-20 | 2024-04-12 | 重庆大学 | Fluorescent color-based oiled paper insulation aging diagnosis method |
| CN113686835A (en) * | 2021-10-11 | 2021-11-23 | 重庆大学 | Method for simultaneously detecting multiple characteristic substances in insulating oil based on liquid-liquid extraction and Raman spectroscopy |
| CN114113030A (en) * | 2021-10-14 | 2022-03-01 | 广东电网有限责任公司广州供电局 | Construction method of analysis model for acetone content in transformer oil and detection method for acetone content |
| CN114113030B (en) * | 2021-10-14 | 2024-07-09 | 广东电网有限责任公司广州供电局 | Construction method of acetone content analysis model in transformer oil and acetone content detection method |
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