CN103185686B - Particulate matter component assay method in transformer oil - Google Patents
Particulate matter component assay method in transformer oil Download PDFInfo
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- CN103185686B CN103185686B CN201110457252.3A CN201110457252A CN103185686B CN 103185686 B CN103185686 B CN 103185686B CN 201110457252 A CN201110457252 A CN 201110457252A CN 103185686 B CN103185686 B CN 103185686B
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- particulate matter
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- resistant container
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Abstract
The present invention provides particulate matter component assay method in a kind of transformer oil, comprises the steps: that taking a certain amount of transformer oil carries out sucking filtration, with the particulate matter on solvent clean filter membrane, is placed in filter membrane in high-temperature resistant container with particulate matter after having cleaned together；Adding butyl acetate in high-temperature resistant container, to dissolve filter membrane, filter membrane dissolves post-heating to remove butyl acetate；In high-temperature resistant container, add Lithium biborate mix with described particulate matter, and cover the Lithium biborate of one layer of equal quality on the mixture, room temperature be progressively warming up to 900～950 DEG C and melt, 15～30 minutes；After being cooled to room temperature, soak in inorganic acid aqueous solution, be heated to 70～90 DEG C, keep 15～30 minutes, move to constant volume in container, use ICP-AES or atomic absorption spectrography (AAS) to quantitative determine.The present invention uses the mode of substep pretreatment, the most time-consuming and energy consumption, and can avoid the medicine using toxicity stronger, only needs single injected sampling to measure and obtains a result.
Description
Technical field
The method of testing of the particulate matter chemical composition that the present invention relates in transformer oil under certain particle diameter.
Background technology
Transformer oil is the compounds such as the one of oil divides gold-plating product, and its main component is alkane, naphthene series's saturated hydrocarbons, aromatic series unsaturated hydrocarbons.Transformator is after being filled with transformer oil, owing to impurity (such as organic polar substances, solid particle polluter, fiber etc.) is dissolved in the oil middle meeting that contacts with solid insulating material and structural material, after energising, oil temperature raises, oil quality deterioration, and it has bigger difference with original transformer oil quality.It is thus desirable to the particulate matter chemical composition in transformer oil is measured.The most not for the chemical element assay method of particulate matter pure in transformer oil, typically measure the coherent element that oil mixes with particulate matter, or with physical means qualitative determination particulate matter component.
Summary of the invention
The present invention provides particulate matter component assay method in a kind of transformer oil, with the drawbacks described above overcoming prior art to exist.
The present invention realizes by the following technical solutions:
Particulate matter component assay method in a kind of transformer oil, comprises the steps:
1, take a certain amount of transformer oil and carry out sucking filtration, with the particulate matter on solvent clean filter membrane, after having cleaned, filter membrane is placed in high-temperature resistant container together with particulate matter；
2, adding butyl acetate in high-temperature resistant container, to dissolve filter membrane, filter membrane dissolves post-heating to remove butyl acetate；
3, in high-temperature resistant container, add Lithium biborate to mix with described particulate matter, and cover the Lithium biborate of one layer of equal quality on the mixture, room temperature be progressively warming up to 900～950 DEG C and melt, 15～30 minutes；
4, after being cooled to room temperature, soak in inorganic acid aqueous solution, be heated to 70～90 DEG C, keep 15～30 minutes, move to constant volume in container, use ICP-AES or atomic absorption spectrography (AAS) to quantitative determine.
Described filter membrane may select product commonly used in the art, preferably cellulose acetate film, and filter sizes is 0.15～5 micron；
The preferred normal heptane of described solvent or petroleum ether；
Described high-temperature resistant container generally can be selected for crucible, preferably platinum crucible, can avoid introducing impurity element interference detection results；
The addition of described butyl acetate is advisable with filter membrane described in proper solubilized, the most also can be suitably excessive, and the heating-up temperature preferably 25～40 DEG C of butyl acetate removed by filter membrane after dissolving；
The mass ratio of described particulate matter and Lithium biborate is 1: 10～20；
Described inorganic acid aqueous solution is hydrochloric acid or salpeter solution, mass concentration preferably 5～10%.
ICP-AES, i.e. ICP-AES (InductivelyCoupledPlasma-AtomicEmissionspectrometry) method, is a kind of spectroscopic analysis methods with induction coupled plasma torch as excitation source.This method has that detection limit is low, accuracy and precision is high, fast, range of linearity width of analyzing speed, and the advantage such as multielement and multiline mensuration simultaneously.Action principle is: sample is lifted into spectrogrph through the peristaltic pump of sampling system, and during by excitation source plasma flare, tested element will be excited by moment, from ground state transition to excited state, is quickly returned to the most again ground state.The most different elements will launch the characteristic light spectral line of different wave length. and the intensity of characteristic light spectral line is directly proportional to the content of element again.Characteristic light spectral line is irradiated on detector after the opticses such as lens, slit, echelle grating, detector become the signal of telecommunication to export spectral line and the intensity-conversion thereof of different characteristic.So can carry out quantitative analysis.
This method is to make solution in pretreatment oil after particulate matter and draw particulate matter component result after mensuration in pertinent instruments, use the mode of substep pretreatment, solve particulate matter component in transformer oil and be difficult to the difficult problem that accurate quantification measures, and owing to only needing step-by-step processing sample, this method is the most time-consuming and energy consumption, and can avoid the medicine (such as Fluohydric acid .) using toxicity stronger；The most only need single injected sampling to measure when measuring on instrument to obtain a result simultaneously.
Detailed description of the invention
Present pre-ferred embodiments is given below, to describe technical scheme in detail.
Taking a certain amount of transformer oil sucking filtration, use bottle,suction during sucking filtration, filter membrane is cellulose acetate film, membrane aperture is 0.45 micron, after the particulate matter on filter membrane reaches 0.1 gram, with solvent clean, solvent selects petroleum ether, after having cleaned, is placed in together in platinum crucible with particulate matter by filter membrane；
Taking 5 milliliters of butyl acetates and dissolve filter membrane in crucible, filter membrane dissolves post-heating and is evaporated butyl acetate to 35 DEG C；
With aerosol sample: Lithium biborate=1: 15 mixing, it is placed in platinum crucible, and covers the Lithium biborate of one layer of isodose on the mixture, Muffle furnace is progressively warming up to by room temperature 900～950 DEG C and melts, keep 15 minutes, take out and be cooled to room temperature；Soak in 10% hydrochloric acid solution, be heated to 80 DEG C, heat while stirring, keep 15 minutes；Move to constant volume in volumetric flask, measure with ICP-AES.The inventive method can accurately measure the composition of particulate matter in transformer oil.
Claims (7)
1. particulate matter component assay method in a transformer oil, it is characterised in that comprise the steps:
1) take a certain amount of transformer oil and carry out sucking filtration, with the particulate matter on solvent clean filter membrane, after having cleaned, filter membrane is placed in high-temperature resistant container together with particulate matter；
2) adding butyl acetate in high-temperature resistant container, to dissolve filter membrane, filter membrane dissolves post-heating to remove butyl acetate；
3) in high-temperature resistant container, add Lithium biborate to mix with described particulate matter, and cover the Lithium biborate of one layer of equal quality on the mixture, room temperature be progressively warming up to 900～950 DEG C and melt, 15～30 minutes；
4) after being cooled to room temperature, soak in inorganic acid aqueous solution, be heated to 70～90 DEG C, keep 15～30 minutes, move to constant volume in container, use ICP-AES or atomic absorption spectrography (AAS) to quantitative determine.
2. the method for claim 1, it is characterised in that described filter membrane is cellulose acetate film, filter sizes is 0.15～5 micron.
3. the method for claim 1, it is characterised in that described solvent is normal heptane or petroleum ether.
4. the method for claim 1, it is characterised in that described high-temperature resistant container is platinum crucible.
5. the method for claim 1, it is characterised in that the heating-up temperature of butyl acetate removed by filter membrane after dissolving be 25～40 DEG C.
6. the method for claim 1, it is characterised in that in described mixture, the mass ratio of particulate matter and Lithium biborate is 1:10～20.
7. the method for claim 1, it is characterised in that described inorganic acid aqueous solution is hydrochloric acid or salpeter solution, mass concentration is 5～10%.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201110457252.3A CN103185686B (en) | 2011-12-30 | 2011-12-30 | Particulate matter component assay method in transformer oil |
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| CN201110457252.3A CN103185686B (en) | 2011-12-30 | 2011-12-30 | Particulate matter component assay method in transformer oil |
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| CN103185686A CN103185686A (en) | 2013-07-03 |
| CN103185686B true CN103185686B (en) | 2016-08-03 |
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Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103364357B (en) * | 2013-08-05 | 2015-04-15 | 国家电网公司 | Detection method for content of trace metal elements in transformer oil by using acid liquor dissolution method to treat transformer oil sample |
| CN104450149B (en) * | 2014-12-17 | 2017-09-29 | 国网上海市电力公司 | A kind of method that particulate matter is extracted in transformer oil |
| CN112924317A (en) * | 2020-12-30 | 2021-06-08 | 广东电网有限责任公司电力科学研究院 | Method for measuring content of free carbon in transformer oil |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5563929A (en) * | 1994-02-18 | 1996-10-08 | The Electric Power Research Institute | On-line monitor for particulate analyte in a moving liquid |
| US6337739B1 (en) * | 1997-04-21 | 2002-01-08 | Fraunhofer-Gesellschaft Zur Foerderung Der Angewandten Forschung E.V. | Method and device for quantitative and qualitative on-line differentiation of biotic and abiotic particles |
| CN101221127A (en) * | 2007-10-26 | 2008-07-16 | 河北省电力研究院 | Concurrent measuring method for multiple metallic elements in transformer oil |
| CN101614656A (en) * | 2008-06-27 | 2009-12-30 | 上海宝钢工业检测公司 | Iron particle and organoferric quantitative analysis method in using lubricating oil |
| CN101923016A (en) * | 2009-06-17 | 2010-12-22 | 华东电力试验研究院有限公司 | Blade deposit sediment measuring method for turbine |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0210265A (en) * | 1988-06-29 | 1990-01-16 | Meidensha Corp | Quantitative analysis method of ni in granulation powder for zno element |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5563929A (en) * | 1994-02-18 | 1996-10-08 | The Electric Power Research Institute | On-line monitor for particulate analyte in a moving liquid |
| US6337739B1 (en) * | 1997-04-21 | 2002-01-08 | Fraunhofer-Gesellschaft Zur Foerderung Der Angewandten Forschung E.V. | Method and device for quantitative and qualitative on-line differentiation of biotic and abiotic particles |
| CN101221127A (en) * | 2007-10-26 | 2008-07-16 | 河北省电力研究院 | Concurrent measuring method for multiple metallic elements in transformer oil |
| CN101614656A (en) * | 2008-06-27 | 2009-12-30 | 上海宝钢工业检测公司 | Iron particle and organoferric quantitative analysis method in using lubricating oil |
| CN101923016A (en) * | 2009-06-17 | 2010-12-22 | 华东电力试验研究院有限公司 | Blade deposit sediment measuring method for turbine |
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