CN113109414B - Method for extracting appearance of iron in transformer oil and measuring content of iron - Google Patents
Method for extracting appearance of iron in transformer oil and measuring content of iron Download PDFInfo
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- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 title claims abstract description 415
- 229910052742 iron Inorganic materials 0.000 title claims abstract description 208
- 238000000034 method Methods 0.000 title claims abstract description 50
- 230000000536 complexating effect Effects 0.000 claims abstract description 30
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 claims abstract description 24
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 11
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000008367 deionised water Substances 0.000 claims abstract description 10
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 10
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 10
- 239000003921 oil Substances 0.000 claims description 94
- 238000000120 microwave digestion Methods 0.000 claims description 10
- 238000005259 measurement Methods 0.000 claims description 7
- 239000010779 crude oil Substances 0.000 claims description 6
- 238000007781 pre-processing Methods 0.000 claims description 6
- 230000008569 process Effects 0.000 claims description 6
- 230000008878 coupling Effects 0.000 claims description 2
- 238000010168 coupling process Methods 0.000 claims description 2
- 238000005859 coupling reaction Methods 0.000 claims description 2
- 230000001939 inductive effect Effects 0.000 claims description 2
- 238000000918 plasma mass spectrometry Methods 0.000 claims description 2
- 238000000605 extraction Methods 0.000 abstract description 12
- 150000002500 ions Chemical class 0.000 abstract description 7
- 238000001514 detection method Methods 0.000 abstract description 5
- 238000003745 diagnosis Methods 0.000 abstract description 5
- 239000000126 substance Substances 0.000 abstract description 5
- 238000004458 analytical method Methods 0.000 abstract description 4
- 229910021432 inorganic complex Inorganic materials 0.000 abstract description 4
- 230000000877 morphologic effect Effects 0.000 abstract description 4
- 238000001095 inductively coupled plasma mass spectrometry Methods 0.000 description 18
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000000705 flame atomic absorption spectrometry Methods 0.000 description 2
- 238000002536 laser-induced breakdown spectroscopy Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000012544 monitoring process Methods 0.000 description 2
- 150000002978 peroxides Chemical class 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 230000002159 abnormal effect Effects 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000004993 emission spectroscopy Methods 0.000 description 1
- 238000009616 inductively coupled plasma Methods 0.000 description 1
- -1 iron ions Chemical class 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000013021 overheating Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000002203 pretreatment Methods 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/62—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/44—Sample treatment involving radiation, e.g. heat
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- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
Abstract
The invention discloses a method for extracting and measuring the occurrence form of iron in transformer oil, which belongs to the technical field of transformer oil detection in oil immersed power transformers, and comprises the steps of extracting free ionic iron in an oil sample by deionized water, and extracting the extracted oil sample by nitric acid to obtain inorganic complex iron; and extracting the organic complex iron by using acetonitrile, wherein the residual oil sample is residual residue iron. The method is based on a continuous extraction technology, and the existing forms of iron are divided into a free ion state, an inorganic complexing state, an organic complexing state and a residue state, so that the method has important significance for evaluating the electrical and chemical properties of the transformer oil; by morphological analysis of occurrence of iron in the transformer oil, theoretical basis is provided for the iron content in the transformer oil as an information carrier for transformer fault diagnosis; the method has the advantages of simple operation, low cost, no secondary pollution and the like.
Description
Technical Field
The invention belongs to the technical field of detection of transformer oil in an oil-immersed power transformer, and particularly relates to a method for extracting an occurrence form of iron in transformer oil and determining the content of the iron in the transformer oil.
Background
The power transformer is used as one of the hub devices of the power grid, and the stable operation of the power transformer is directly related to the power supply reliability of the power system. The transformer oil has the functions of insulating, cooling, arc extinguishing and information carrier, and the performance of the transformer oil is directly related to the safe and stable operation of the transformer. Iron materials in the oil immersed power transformer cause iron corrosion and melting loss to be aggravated when abnormal operations such as overheating or discharging occur. The method closely pays attention to the content of trace iron in the transformer oil, is helpful for monitoring or accurately judging potential hidden hazards and fault positions of the transformer, and has important significance for safe and stable operation of the transformer.
In recent years, iron content in transformer oil and occurrence of morphological problems have been paid attention to. The inherent polar substances in the transformer oil and free radicals generated in the initial oxidation stage attack the surface of the iron material, and different occurrence forms of iron are formed, such as a free ion state, an inorganic complex state, an organic complex state, a residue state and the like, the occurrence forms of different iron establish stable dynamic balance in the oil, for example, when peroxide in the oil exists in a large amount, the peroxide reacts with the free ion state to generate a stable organic complex state, and acidic substances generated in the reaction process accelerate the conversion of the inorganic iron to the free ion state.
Currently, methods for detecting the iron content in transformer oil include Flame Atomic Absorption Spectrometry (FAAS), inductively coupled plasma emission spectrometry (ICP-AES), laser Induced Breakdown Spectrometry (LIBS), inductively coupled plasma mass spectrometry (ICP-MS) and the like, and the detection means have the advantages of high sensitivity, wide linear range, low detection limit and the like, however, due to the limitation of a pretreatment method, only the information of the total iron content in the oil product can be provided, and the analysis results of the content and the change trend of different iron occurrence forms are lacking. The method for monitoring the iron content and occurrence form of the transformer oil can accurately reflect the service performance of the transformer oil, and can know the running state of the transformer, so that the method has important practical significance for implementing an effective power transformer fault diagnosis technology.
Disclosure of Invention
The invention aims to solve the existing technical problems and provide an extraction method of the occurrence forms of iron in transformer oil and a content determination method thereof, which realize quantitative determination of different occurrence forms of iron in the transformer oil by means of graded continuous extraction and are used for perfecting the defects of the existing iron detection technology in the transformer oil so as to provide theoretical basis for the iron content in the transformer oil as an information carrier for transformer fault diagnosis.
In order to achieve the above purpose, the invention adopts the following technical scheme: the method for extracting the appearance of iron in the transformer oil and determining the content thereof is characterized by comprising the following steps in sequence:
step 1: placing 20mL of oil sample into a 50mL volumetric flask, adding 10 mL-20 mL of deionized water, and placing the volumetric flask into a shaking table at 50 ℃ to shake for 3h at 300 r/min; centrifuging the oscillated sample at a rotation speed of 5000r/min for 10min, and taking an upper layer oil sample as a sample A to be detected;
step 2: placing 10mL of the upper layer oil sample in the step 1 into a 20mL volumetric flask, adding 6 mL-10 mL of nitric acid solution, and placing the volumetric flask into a shaking table at 80 ℃ to shake for 1h at 200 r/min; centrifuging the oscillated sample at a rotation speed of 5000r/min for 10min, and taking an upper layer oil sample as a sample B to be detected;
step 3: placing 5mL of the upper layer oil sample in the step 2 into a 10mL volumetric flask, adding 3 mL-5 mL of AR grade acetonitrile, and placing the volumetric flask into a shaking table at 60 ℃ to shake for 2h at 200 r/min; centrifuging the oscillated sample at a rotation speed of 5000r/min for 10min, and taking an upper layer oil sample as a sample C to be detected;
step 4: taking the crude oil sample in the step 1 to measure the total iron content, obtaining the total iron content, wherein the free ionic iron content is the difference between the total iron content and the iron content of the sample A to be measured, the inorganic complexing iron content is the difference between the iron content of the sample A to be measured and the iron content of the sample B to be measured, the organic complexing iron content is the difference between the iron content of the sample B to be measured and the iron content of the sample C to be measured, and the residue iron content is the difference between the total iron content and the sum of the free ionic iron content, the inorganic complexing iron content and the organic complexing iron content, so as to realize quantitative measurement of different iron occurrence forms in transformer oil.
Further, the mass concentration of the nitric acid solution is 20% -40%.
Further, the measuring process of the iron content, the iron content of the sample to be measured A, the iron content of the sample to be measured B and the iron content of the sample to be measured C is as follows: and respectively preprocessing the oil sample, the sample A to be detected, the sample B to be detected and the sample C to be detected by adopting a microwave digestion method, and measuring the iron content of the processed samples by utilizing an inductive coupling plasma mass spectrometry method to respectively obtain the total iron content, the iron content of the sample A to be detected, the iron content of the sample B to be detected and the iron content of the sample C to be detected.
Through the design scheme, the invention has the following beneficial effects:
1. based on the continuous extraction technology, the existing forms of iron are divided into a free ion state, an inorganic complexing state, an organic complexing state and a residue state, and the method has important significance for evaluating the electrical and chemical properties of the transformer oil.
2. By morphological analysis of occurrence of iron in the transformer oil, theoretical basis is provided for the iron content in the transformer oil as an information carrier for transformer fault diagnosis.
3. The method has the advantages of simple operation, low cost, no secondary pollution and the like.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and constitute a part of this application, illustrate embodiments of the invention and together with the description serve to explain the invention and do not constitute a undue limitation of the invention, and in which:
FIG. 1 is a flow chart of continuous extraction of transformer oil in the invention.
Detailed Description
Referring to fig. 1, the invention provides a method for extracting and measuring the content of iron in transformer oil, which divides the iron appearance into free ion state, inorganic complex state, organic complex state and residue state by a grading continuous extraction technology, and realizes quantitative measurement of different iron appearance in transformer oil, and the method specifically comprises the following steps:
step 1: placing 20mL of oil sample into a 50mL volumetric flask, adding 10 mL-20 mL of deionized water, and placing the volumetric flask into a shaking table at 50 ℃ to shake for 3h at 300 r/min; centrifuging the oscillated sample at a rotation speed of 5000r/min for 10min, taking an upper layer oil sample as a sample A to be detected, and extracting free ionic iron in the oil sample by using deionized water;
step 2: placing 10mL of the upper layer oil sample in the step 1 into a 20mL volumetric flask, adding 6 mL-10 mL of nitric acid solution with the mass concentration of 20% -40%, and placing the volumetric flask into a shaking table at 80 ℃ to shake for 1h at 200 r/min; centrifuging the oscillated sample at a rotation speed of 5000r/min for 10min, and taking an upper layer oil sample as a sample B to be detected;
step 3: placing 5mL of the upper layer oil sample in the step 2 into a 10mL volumetric flask, adding 3 mL-5 mL of AR grade acetonitrile, and placing the volumetric flask into a shaking table at 60 ℃ to shake for 2h at 200 r/min; centrifuging the oscillated sample at a rotation speed of 5000r/min for 10min, and taking an upper layer oil sample as a sample C to be detected;
step 4: taking the crude oil sample in the step 1 to measure the total iron content, obtaining the total iron content, wherein the free ionic iron content is the difference between the total iron content and the iron content of the sample A to be measured, the inorganic complexing iron content is the difference between the iron content of the sample A to be measured and the iron content of the sample B to be measured, the organic complexing iron content is the difference between the iron content of the sample B to be measured and the iron content of the sample C to be measured, and the residue iron content is the difference between the total iron content and the sum of the free ionic iron content, the inorganic complexing iron content and the organic complexing iron content, so as to realize quantitative measurement of different iron occurrence forms in transformer oil.
Wherein: the determination process of the total iron content is as follows: pretreating an oil sample by adopting a microwave digestion method, and measuring the iron content of the treated sample by utilizing an inductively coupled plasma mass spectrometry (ICP-MS) to obtain the total iron content;
and similarly, respectively preprocessing the sample A to be detected, the sample B to be detected and the sample C to be detected by adopting a microwave digestion method, and measuring the iron content of the processed samples by utilizing an inductively coupled plasma mass spectrometry (ICP-MS) so as to obtain the iron content of the sample A to be detected, the iron content of the sample B to be detected and the iron content of the sample C to be detected.
Based on the occurrence forms and the content of iron in the accident transformer, the invention adopts a continuous extraction method to extract different occurrence forms of iron, realizes the complete extraction of different occurrence forms of iron by controlling the ratio of extractant to oil sample at each level and the extraction and separation conditions, takes the extraction of free ionic iron as an example, controls the oil-water ratio to be 1 (0.5-1), oscillates for 3 hours at the constant temperature of 50 ℃ for 300r/min, and carries out centrifugal separation for 10min at 5000r/min, and the free iron ions in the oil sample can completely enter into the deionized water of the extraction phase.
The present invention will be described in detail with reference to specific examples below in order to make the objects, features, and advantages of the present invention more apparent and understandable. It should be noted that the following examples are illustrative, not limiting, and are not intended to limit the scope of the invention as claimed. The starting materials used in the examples were all commercially available products. Well-known methods, procedures, and flows have not been described in detail so as not to obscure the nature of the invention.
Example 1
The method for extracting the occurrence form of the iron in the transformer oil and measuring the content of the iron in the transformer oil in the embodiment comprises the following steps:
step 1: placing 20mL of oil sample into a 50mL volumetric flask, adding 10mL of deionized water, and placing the volumetric flask into a shaking table at 50 ℃ to shake for 3h at 300 r/min; centrifuging the oscillated sample at a rotation speed of 5000r/min for 10min, and taking an upper layer oil sample as a sample A to be detected;
step 2: placing 10mL of the upper layer oil sample in the step 1 into a 20mL volumetric flask, adding 6mL of nitric acid solution with the mass concentration of 40%, and placing the volumetric flask into a shaking table at 80 ℃ to shake for 1h at 200 r/min; centrifuging the oscillated sample at a rotation speed of 5000r/min for 10min, and taking an upper layer oil sample as a sample B to be detected;
step 3: placing 5mL of the upper layer oil sample in the step 2 into a 10mL volumetric flask, adding 3mL of AR grade acetonitrile, and placing the volumetric flask into a shaking table at 60 ℃ to shake for 2h at 200 r/min; centrifuging the oscillated sample at a rotation speed of 5000r/min for 10min, and taking an upper layer oil sample as a sample C to be detected;
step 4: taking the crude oil sample in the step 1 to measure the total iron content, obtaining the total iron content, wherein the free ionic iron content is the difference between the total iron content and the iron content of a sample to be measured, the inorganic complexing iron content is the difference between the iron content of a sample to be measured and the iron content of a sample to be measured, the organic complexing iron content is the difference between the iron content of a sample to be measured and the iron content of a sample to be measured C, and the residue iron content is the difference between the total iron content and the sum of the free ionic iron content, the inorganic complexing iron content and the organic complexing iron content, wherein: the determination process of the total iron content is as follows: pretreating an oil sample by adopting a microwave digestion method, and measuring the iron content of the treated sample by utilizing an inductively coupled plasma mass spectrometry (ICP-MS) to obtain the total iron content; and similarly, respectively preprocessing a to-be-detected sample A, a to-be-detected sample B and a to-be-detected sample C by adopting a microwave digestion method, and measuring the iron content of the processed samples by utilizing an inductively coupled plasma mass spectrometry (ICP-MS) to obtain the iron content of the to-be-detected sample A, the iron content of the to-be-detected sample B and the iron content of the to-be-detected sample C, thereby realizing quantitative measurement of different iron occurrence forms in transformer oil.
Example 2
The method for extracting the occurrence form of the iron in the transformer oil and measuring the content of the iron in the transformer oil in the embodiment comprises the following steps:
step 1: placing 20mL of oil sample into a 50mL volumetric flask, adding 15mL of deionized water, and placing the volumetric flask into a shaking table at 50 ℃ to shake for 3h at 300 r/min; centrifuging the oscillated sample at a rotation speed of 5000r/min for 10min, and taking an upper layer oil sample as a sample A to be detected;
step 2: placing 10mL of the upper layer oil sample in the step 1 into a 20mL volumetric flask, adding 8mL of a nitric acid solution with the mass concentration of 30%, and placing the volumetric flask into a shaking table at 80 ℃ to shake for 1h at 200 r/min; centrifuging the oscillated sample at a rotation speed of 5000r/min for 10min, and taking an upper layer oil sample as a sample B to be detected;
step 3: placing 5mL of the upper layer oil sample in the step 2 into a 10mL volumetric flask, adding 4mL of AR grade acetonitrile, and placing the volumetric flask into a shaking table at 60 ℃ to shake for 2h at 200 r/min; centrifuging the oscillated sample at a rotation speed of 5000r/min for 10min, and taking an upper layer oil sample as a sample C to be detected;
step 4: taking the crude oil sample in the step 1 to measure the total iron content, obtaining the total iron content, wherein the free ionic iron content is the difference between the total iron content and the iron content of a sample to be measured, the inorganic complexing iron content is the difference between the iron content of a sample to be measured and the iron content of a sample to be measured, the organic complexing iron content is the difference between the iron content of a sample to be measured and the iron content of a sample to be measured C, and the residue iron content is the difference between the total iron content and the sum of the free ionic iron content, the inorganic complexing iron content and the organic complexing iron content, wherein: the determination process of the total iron content is as follows: pretreating an oil sample by adopting a microwave digestion method, and measuring the iron content of the treated sample by utilizing an inductively coupled plasma mass spectrometry (ICP-MS) to obtain the total iron content; and similarly, respectively preprocessing a to-be-detected sample A, a to-be-detected sample B and a to-be-detected sample C by adopting a microwave digestion method, and measuring the iron content of the processed samples by utilizing an inductively coupled plasma mass spectrometry (ICP-MS) to obtain the iron content of the to-be-detected sample A, the iron content of the to-be-detected sample B and the iron content of the to-be-detected sample C, thereby realizing quantitative measurement of different iron occurrence forms in transformer oil.
Example 3
The method for extracting the occurrence form of the iron in the transformer oil and measuring the content of the iron in the transformer oil in the embodiment comprises the following steps:
step 1: placing 20mL of oil sample into a 50mL volumetric flask, adding 20mL of deionized water, and placing the volumetric flask into a shaking table at 50 ℃ to shake for 3h at 300 r/min; centrifuging the oscillated sample at a rotation speed of 5000r/min for 10min, and taking an upper layer oil sample as a sample A to be detected;
step 2: placing 10mL of the upper layer oil sample in the step 1 into a 20mL volumetric flask, adding 10mL of nitric acid solution with the mass concentration of 20%, and placing the volumetric flask into a shaking table at 80 ℃ to shake for 1h at 200 r/min; centrifuging the oscillated sample at a rotation speed of 5000r/min for 10min, and taking an upper layer oil sample as a sample B to be detected;
step 3: placing 5mL of the upper layer oil sample in the step 2 into a 10mL volumetric flask, adding 5mL of AR grade acetonitrile, and placing the volumetric flask into a shaking table at 60 ℃ to shake for 2h at 200 r/min; centrifuging the oscillated sample at a rotation speed of 5000r/min for 10min, and taking an upper layer oil sample as a sample C to be detected;
step 4: taking the crude oil sample in the step 1 to measure the total iron content, obtaining the total iron content, wherein the free ionic iron content is the difference between the total iron content and the iron content of a sample to be measured, the inorganic complexing iron content is the difference between the iron content of a sample to be measured and the iron content of a sample to be measured, the organic complexing iron content is the difference between the iron content of a sample to be measured and the iron content of a sample to be measured C, and the residue iron content is the difference between the total iron content and the sum of the free ionic iron content, the inorganic complexing iron content and the organic complexing iron content, wherein: the determination process of the total iron content is as follows: pretreating an oil sample by adopting a microwave digestion method, and measuring the iron content of the treated sample by utilizing an inductively coupled plasma mass spectrometry (ICP-MS) to obtain the total iron content; and similarly, respectively preprocessing a to-be-detected sample A, a to-be-detected sample B and a to-be-detected sample C by adopting a microwave digestion method, and measuring the iron content of the processed samples by utilizing an inductively coupled plasma mass spectrometry (ICP-MS) to obtain the iron content of the to-be-detected sample A, the iron content of the to-be-detected sample B and the iron content of the to-be-detected sample C, thereby realizing quantitative measurement of different iron occurrence forms in transformer oil.
In summary, according to the method for extracting the occurrence form of iron in the transformer oil and the content measuring method thereof, deionized water is utilized to extract free ionic iron in an oil sample, and nitric acid is utilized to extract the extracted oil sample, so that inorganic complex iron is obtained; and extracting the organic complex iron by using acetonitrile, wherein the residual oil sample is residual residue iron. The method is based on a continuous extraction technology, and the existing forms of iron are divided into a free ion state, an inorganic complexing state, an organic complexing state and a residue state, so that the method has important significance for evaluating the electrical and chemical properties of the transformer oil; by morphological analysis of occurrence of iron in the transformer oil, theoretical basis is provided for the iron content in the transformer oil as an information carrier for transformer fault diagnosis; the method has the advantages of simple operation, low cost, no secondary pollution and the like.
Claims (3)
1. The method for extracting the appearance of iron in the transformer oil and determining the content thereof is characterized by comprising the following steps in sequence:
step 1: placing 20mL of oil sample into a 50mL volumetric flask, adding 10 mL-20 mL of deionized water, and placing the volumetric flask into a shaking table at 50 ℃ to shake for 3h at 300 r/min; centrifuging the oscillated sample at a rotation speed of 5000r/min for 10min, and taking an upper layer oil sample as a sample A to be detected;
step 2: placing 10mL of the upper layer oil sample in the step 1 into a 20mL volumetric flask, adding 6 mL-10 mL of nitric acid solution, and placing the volumetric flask into a shaking table at 80 ℃ to shake for 1h at 200 r/min; centrifuging the oscillated sample at a rotation speed of 5000r/min for 10min, and taking an upper layer oil sample as a sample B to be detected;
step 3: placing 5mL of the upper layer oil sample in the step 2 into a 10mL volumetric flask, adding 3 mL-5 mL of AR grade acetonitrile, and placing the volumetric flask into a shaking table at 60 ℃ to shake for 2h at 200 r/min; centrifuging the oscillated sample at a rotation speed of 5000r/min for 10min, and taking an upper layer oil sample as a sample C to be detected;
step 4: taking the crude oil sample in the step 1 to measure the total iron content, obtaining the total iron content, wherein the free ionic iron content is the difference between the total iron content and the iron content of the sample A to be measured, the inorganic complexing iron content is the difference between the iron content of the sample A to be measured and the iron content of the sample B to be measured, the organic complexing iron content is the difference between the iron content of the sample B to be measured and the iron content of the sample C to be measured, and the residue iron content is the difference between the total iron content and the sum of the free ionic iron content, the inorganic complexing iron content and the organic complexing iron content, so as to realize quantitative measurement of different iron occurrence forms in transformer oil.
2. The method for extracting the appearance of iron in transformer oil and determining the content thereof according to claim 1, wherein the method comprises the following steps: the mass concentration of the nitric acid solution is 20% -40%.
3. The method for extracting the appearance of iron in transformer oil and determining the content thereof according to claim 1, wherein the method comprises the following steps: the measuring process of the iron content, the iron content of the sample A to be measured, the iron content of the sample B to be measured and the iron content of the sample C to be measured is as follows: and respectively preprocessing the oil sample, the sample A to be detected, the sample B to be detected and the sample C to be detected by adopting a microwave digestion method, and measuring the iron content of the processed samples by utilizing an inductive coupling plasma mass spectrometry method to respectively obtain the total iron content, the iron content of the sample A to be detected, the iron content of the sample B to be detected and the iron content of the sample C to be detected.
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