CN115032112A - Method for measuring free carbon content of transformer oil - Google Patents

Method for measuring free carbon content of transformer oil Download PDF

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CN115032112A
CN115032112A CN202210644856.7A CN202210644856A CN115032112A CN 115032112 A CN115032112 A CN 115032112A CN 202210644856 A CN202210644856 A CN 202210644856A CN 115032112 A CN115032112 A CN 115032112A
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mixed solution
transformer oil
preset volume
weight
solid powder
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张丽
李智
付强
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Guangdong Power Grid Co Ltd
Electric Power Research Institute of Guangdong Power Grid Co Ltd
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Guangdong Power Grid Co Ltd
Electric Power Research Institute of Guangdong Power Grid Co Ltd
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N5/00Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid
    • G01N5/04Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid by removing a component, e.g. by evaporation, and weighing the remainder
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/34Purifying; Cleaning
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/38Diluting, dispersing or mixing samples
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/40Concentrating samples
    • G01N1/4077Concentrating samples by other techniques involving separation of suspended solids
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/40Concentrating samples
    • G01N1/4077Concentrating samples by other techniques involving separation of suspended solids
    • G01N2001/4094Concentrating samples by other techniques involving separation of suspended solids using ultrasound

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Abstract

The invention discloses a method for measuring the free carbon content of transformer oil, which comprises the steps of carrying out centrifugal treatment on a first mixed solution obtained based on the transformer oil and petroleum ether to obtain a second mixed solution; adding petroleum ether into the second mixed solution to obtain a third mixed solution, performing ultrasonic treatment, air drying and drying treatment on the third mixed solution to obtain a first solid powder substance and a first weight thereof, performing organic component cracking treatment on the first solid powder substance to obtain a second solid powder substance and a second weight thereof, performing combustion treatment on the second solid powder substance to obtain a third solid powder substance and a third weight thereof, calculating a first difference value between the second weight and the third weight, taking the first difference value as a weight value of free carbon in the transformer oil, and calculating the content of the free carbon based on the transformer oil with a first preset volume. Compared with the prior art, the method can improve the efficiency and accuracy of measuring the content of free carbon in the transformer oil.

Description

Method for measuring free carbon content of transformer oil
Technical Field
The invention relates to the technical field of free carbon content determination, in particular to a method for determining the free carbon content of transformer oil.
Background
Transformer oil is a liquid medium with cooling, arc-extinguishing and insulating functions. The excellent oil performance of the transformer is an important guarantee for the safe and stable operation of the transformer. After the large transformer is put into operation, the service life of the transformer is as long as thirty-four years, but free carbon can be generated due to long-term effects of local high temperature, arc extinction and the like of transformer oil, the free carbon belongs to conductive substances, and a conductive small bridge is easily formed under the action of an electric field, so that insulation breakdown is caused, equipment faults are caused, and the method for measuring the content of the free carbon in the transformer oil is particularly important.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: the method for measuring the free carbon content of the transformer oil can improve the efficiency and accuracy of measuring the free carbon content in the transformer oil.
In order to solve the technical problem, the invention provides a method for measuring the content of free carbon in transformer oil, which comprises the following steps:
mixing and shaking up transformer oil with a first preset volume and petroleum ether with a second preset volume to obtain a first mixed solution, and carrying out air release treatment on a centrifuge tube filled with the first mixed solution;
centrifuging the centrifuge tube to separate supernatant liquid from the first mixed solution, taking the residual substances in the centrifuge tube as a second mixed solution, and centrifuging the second mixed solution for a preset number of times to obtain a third mixed solution;
adding petroleum ether with a third preset volume into the third mixed solution to obtain a fourth mixed solution, and carrying out ultrasonic treatment on a centrifugal tube filled with the fourth mixed solution;
transferring the fourth mixed solution after ultrasonic treatment to a watch glass, carrying out air drying treatment on the fourth mixed solution in the watch glass to volatilize petroleum ether in the fourth mixed solution, drying the watch glass to obtain a first solid powder substance, and obtaining a first weight of the first solid powder substance;
placing the first solid powder substance in a thermogravimetric analyzer so that the thermogravimetric analyzer conducts organic component cracking treatment on the first solid powder substance in a nitrogen flow mode to obtain a second solid powder substance, and obtaining a second weight of the second solid powder substance; enabling the thermogravimetric analyzer to perform combustion treatment on the second solid powder substance in an oxygen flow mode to obtain a third solid powder substance and obtain a third weight of the third solid powder substance;
and calculating a first difference value between the second weight and the third weight, taking the first difference value as a weight value of free carbon in the transformer oil, and calculating the content of the free carbon based on the first preset volume of the transformer oil.
As a possible implementation manner, after obtaining the second weight of the solid powder substance after combustion, the method further includes:
calculating a second difference value between the first weight and the second weight, taking the second difference value as a weight value of the component in the transformer oil, and calculating the content of the component based on the first preset volume of the transformer oil;
taking the third weight of the third solid powder substance as the weight of the inorganic components in the transformer oil, and calculating the content of the inorganic components based on the first preset volume of the transformer oil.
As a possible implementation manner, the centrifugation treatment is performed on the second mixed solution for a preset number of times to obtain a third mixed solution, and the method specifically includes:
obtaining petroleum ether with a second preset volume, mixing and shaking the petroleum ether with the second preset volume and the second mixed solution to obtain a fifth mixed solution, and carrying out air release treatment on a centrifuge tube filled with the fifth mixed solution;
centrifuging the centrifuge tube filled with the fifth mixed solution to separate supernatant from the fifth mixed solution, taking the residual substances in the centrifuge tube as a sixth mixed solution,
obtaining petroleum ether with a second preset volume again, mixing and shaking the petroleum ether with the second preset volume and the sixth mixed solution to obtain a seventh mixed solution, and carrying out air release treatment on the centrifuge tube filled with the seventh mixed solution;
and centrifuging the centrifuge tube filled with the seventh mixed solution to separate supernatant liquid from the seventh mixed solution, and taking the residual substances in the centrifuge tube as a third mixed solution.
As a possible implementation manner, after the fourth mixed liquid after the ultrasonic treatment is transferred to the watch glass, the method further includes:
the method comprises the steps of obtaining petroleum ether with a fourth preset volume, adding the petroleum ether with the fourth preset volume into a centrifuge tube filled with a fourth mixed liquid, so that the centrifuge tube is cleaned by the petroleum ether with the fourth preset volume, and transferring all substances in the centrifuge tube into a watch glass after cleaning, wherein the value range of the fourth preset volume is 1-3 ml.
As a possible implementation, the petroleum ether may be provided as n-hexane.
As a possible implementation manner, a value range of the first preset volume is 5-25 ml, a value range of the second preset volume is 5-25 ml, and a value range of a volume ratio of the first preset volume to the second preset volume is 1: 1-1: 5;
the value range of the third preset volume is 1-3 ml.
As a possible implementation manner, the parameter setting of the thermogravimetric analyzer in the nitrogen flow rate mode includes: setting the value range of nitrogen flow to be 30-50 ml/min, setting the value range of heating rate to be 10-20K/min, setting the value range of heating amplitude to be 40 +/-10 ℃ to 500 +/-50 ℃, and setting the value range of constant temperature time to be 500 +/-50 ℃ for 5-10 minutes.
As a possible implementation manner, the parameter setting of the thermogravimetric analyzer in the oxygen flow rate mode includes: setting the value range of oxygen flow to be 30-50 ml/min, setting the value range of temperature rise rate to be 10-20K/min, and setting the value range of temperature rise amplitude to be 500 +/-50 ℃ to 700 +/-50 ℃.
As a possible implementation manner, the centrifugal tube filled with the third mixed liquid is subjected to ultrasonic treatment, and the value range of the set ultrasonic time is 1-3 minutes.
As a possible implementation manner, the watch glass is dried, and the set drying temperature is in the range of 40-60 ℃.
Compared with the prior art, the method for measuring the free carbon content of the transformer oil has the following beneficial effects:
mixing and shaking up transformer oil with a first preset volume and petroleum ether with a second preset volume to obtain a first mixed solution, and carrying out air release treatment on a centrifugal tube filled with the first mixed solution; centrifuging the centrifuge tube to separate supernatant liquid from the first mixed solution, taking the residual substances in the centrifuge tube as a second mixed solution, and centrifuging the second mixed solution for a preset number of times to obtain a third mixed solution; adding petroleum ether with a third preset volume into the third mixed solution to obtain a fourth mixed solution, and carrying out ultrasonic treatment on a centrifugal tube filled with the fourth mixed solution; transferring the fourth mixed solution after ultrasonic treatment to a watch glass, carrying out air drying treatment on the fourth mixed solution in the watch glass to volatilize petroleum ether in the fourth mixed solution, drying the watch glass to obtain a first solid powder substance, and obtaining a first weight of the first solid powder substance; placing the first solid powder substance in a thermogravimetric analyzer so that the thermogravimetric analyzer conducts organic component cracking treatment on the first solid powder substance in a nitrogen flow mode to obtain a second solid powder substance, and obtaining a second weight of the second solid powder substance; enabling the thermogravimetric analyzer to perform combustion treatment on the second solid powder substance in an oxygen flow mode to obtain a third solid powder substance and obtain a third weight of the third solid powder substance; and calculating a first difference value between the second weight and the third weight, taking the first difference value as a weight value of free carbon in the transformer oil, and calculating the content of the free carbon based on the first preset volume of the transformer oil. Compared with the prior art, the technical scheme of the invention can improve the efficiency and accuracy of measuring the content of the free carbon in the transformer oil, and the measuring process of the content of the free carbon is simple and convenient to operate.
Drawings
Fig. 1 is a schematic flow chart of an embodiment of a method for measuring the free carbon content of transformer oil according to the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the present application, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
Referring to fig. 1, fig. 1 is a schematic flow chart of an embodiment of a method for measuring the free carbon content of transformer oil according to the present invention, as shown in fig. 1, the method includes steps 101 to 106, specifically as follows:
step 101: mixing and shaking up the transformer oil with the first preset volume and the petroleum ether with the second preset volume to obtain a first mixed solution, and carrying out air release treatment on a centrifugal tube filled with the first mixed solution.
In an embodiment, the measuring cylinder is used for accurately measuring the transformer oil with the first preset volume and the petroleum ether with the second preset volume respectively, and the transformer oil with the first preset volume and the petroleum ether with the second preset volume are poured into the centrifuge tube to be mixed and shaken up, namely, the centrifuge tube with the first mixed liquid is deflated, namely, the cover of the centrifuge tube is opened to deflate.
In one embodiment, before the transformer oil is measured by the measuring cylinder, the transformer oil needs to be shaken up, so that free carbon in the transformer oil is prevented from being deposited at the bottom of a glass bottle for loading the transformer oil, the free carbon can be uniformly distributed in the transformer oil, and the accuracy of subsequent detection of the content of the free carbon is improved.
In one embodiment, a value range of the first preset volume is 5-25 ml, a value range of the second preset volume is 5-25 ml, and a volume ratio of the first preset volume to the second preset volume is 1: 1-1: and 5, based on the first preset volume and the second preset volume, selecting the capacity of the centrifuge tube loaded with the first mixed solution within the range of 50-100 ml.
In one embodiment, a second predetermined volume of petroleum ether can be exchanged for a second predetermined volume of n-hexane, and the remaining steps are as described above.
Step 102: and centrifuging the centrifuge tube to separate supernatant liquid from the first mixed solution, taking the residual substances in the centrifuge tube as second mixed solution, and centrifuging the second mixed solution for preset times to obtain third mixed solution.
In one embodiment, put into centrifuge after covering the centrifuging tube lid that will be equipped with first mixed liquid and carry out centrifugal treatment, wherein, set up to centrifuge's parameter: the value range of the rotation rate is set to be 2500 rpm-5000 rpm, and the value range of the set centrifugal time is as follows: 3-5 minutes.
In one embodiment, after the centrifugation, the supernatant of the first mixture liquid is separated from the centrifuge tube, the centrifuge tube is taken out of the centrifuge, the separated supernatant of the centrifuge tube is removed, and the remaining substances in the centrifuge tube are used as the second mixture liquid.
In one embodiment, the second mixed solution is centrifuged for a predetermined number of times to obtain a third mixed solution, so as to ensure that the transformer oil in the centrifugal tube is completely cleaned, wherein the predetermined number of times is two.
Specifically, a second preset volume of petroleum ether is obtained, the second preset volume of petroleum ether and a second mixed solution are mixed and shaken up to obtain a fifth mixed solution, and a centrifugal tube filled with the fifth mixed solution is subjected to air release treatment; centrifuging the centrifuge tube filled with the fifth mixed solution to separate supernatant from the fifth mixed solution, taking the residual substances in the centrifuge tube as a sixth mixed solution, obtaining petroleum ether with a second preset volume again, mixing the petroleum ether with the second preset volume with the sixth mixed solution, shaking up to obtain a seventh mixed solution, and degassing the centrifuge tube filled with the seventh mixed solution; and centrifuging the centrifuge tube filled with the seventh mixed solution to separate supernatant liquid from the seventh mixed solution, and taking the residual substances in the centrifuge tube as a third mixed solution.
Step 103: and adding petroleum ether with a third preset volume into the third mixed solution to obtain a fourth mixed solution, and carrying out ultrasonic treatment on the centrifuge tube filled with the fourth mixed solution.
In one embodiment, a third preset volume of petroleum ether is added into a centrifuge tube filled with a third mixed solution after two times of centrifugation to obtain a fourth mixed solution, and the fourth mixed solution is subjected to ultrasonic treatment so as to uniformly disperse substances deposited at the bottom of the centrifuge tube in the centrifuge tube, wherein the selected range of the set ultrasonic treatment time is 1-3 minutes.
In one embodiment, the third predetermined volume is selected from the range of 1-3 ml.
Step 104: and transferring the fourth mixed solution after ultrasonic treatment to a watch glass, carrying out air drying treatment on the fourth mixed solution in the watch glass to volatilize petroleum ether in the fourth mixed solution, drying the watch glass to obtain a first solid powder substance, and obtaining the first weight of the first solid powder substance.
In one embodiment, the fourth mixed solution loaded in the centrifuge tube is also transferred to the watch glass after the ultrasonic treatment is finished.
In one embodiment, after transferring the fourth mixture to the watch glass, the centrifuge tube is washed with a fourth predetermined volume of petroleum ether to ensure that all the contents of the centrifuge tube are transferred to the watch glass.
Specifically, the method comprises the following steps: the petroleum ether of the fourth preset volume is obtained, the petroleum ether of the fourth preset volume is added into the centrifugal tube filled with the fourth mixed liquid, so that the petroleum ether of the fourth preset volume is right for cleaning the centrifugal tube, and after cleaning, all substances in the centrifugal tube are transferred to the watch glass. Wherein the fourth preset volume is selected within the range of 1-3 ml.
In one embodiment, the petri dish is placed in a fume hood to allow the fourth mixed solution on the petri dish to be air-dried, i.e., the petroleum ether in the fourth mixed solution is volatilized until all the petroleum ether in the fourth mixed solution is volatilized to be dry.
In an embodiment, after the petroleum ether is volatilized to be dried, the current fourth mixed liquid on the watch glass is dried, that is, the watch glass is placed in an oven, the drying temperature is set to be in a range of 40-60 ℃, so that the fourth mixed liquid in the watch glass is dried into the first solid powder substance, and the first solid powder substance is weighed based on a balance scale to obtain the first weight of the first solid powder substance.
Step 105: placing the first solid powder substance in a thermogravimetric analyzer so that the thermogravimetric analyzer conducts organic component cracking treatment on the first solid powder substance in a nitrogen flow mode to obtain a second solid powder substance, and obtaining a second weight of the second solid powder substance; and burning the second solid powder substance by the thermogravimetric analyzer in an oxygen flow mode to obtain a third solid powder substance and obtain a third weight of the third solid powder substance.
In one embodiment, the parameter setting of the thermogravimetric analyzer in the oxygen flow mode includes: setting the value range of oxygen flow to be 30-50 ml/min, setting the value range of temperature rise rate to be 10-20K/min, and setting the value range of temperature rise amplitude to be 500 +/-50 ℃ to 700 +/-50 ℃.
In one embodiment, the parameter settings of the thermogravimetric analyzer in nitrogen flow mode include: setting the value range of nitrogen flow to be 30-50 ml/min, setting the value range of heating rate to be 10-20K/min, setting the value range of heating amplitude to be 40 +/-10 ℃ to 500 +/-50 ℃, and setting the value range of constant temperature time to be 500 +/-50 ℃ for 5-10 minutes.
In one embodiment, the thermogravimetric analyzer is heated to 500 ℃ ± 50 ℃ in nitrogen flow mode to crack the organic components in the transformer oil, comprising: transformer oil molecules, insulating paper fibers and other composite organic materials used inside the transformer, such as insulating paint, composite wrapping tape and the like, are dissolved in the transformer oil. Therefore, in the present example, the organic component in the first solid powder substance was removed based on the organic component cracking treatment, and the first solid powder substance containing no organic component was used as the second solid powder substance.
In one embodiment, the thermogravimetric analyzer heats up to 700 ℃ ± 50 ℃ in the oxygen flow mode to combust the free carbon, and the reduced weight is the weight of the free carbon, so that in this embodiment, the free carbon in the second solid powder is removed based on the combustion process, and the second solid powder substance from which the free carbon is removed is used as the third solid powder substance.
Step 106: and calculating a first difference value between the second weight and the third weight, taking the first difference value as a weight value of free carbon in the transformer oil, and calculating the content of the free carbon based on the first preset volume of the transformer oil.
In one embodiment, the first weight includes organic components, free carbon and inorganic components of the transformer oil, the second weight includes free carbon and inorganic components of the transformer oil, and the third weight includes inorganic components of the transformer oil.
In an embodiment, a first difference between the second weight and the third weight is calculated, that is, a difference obtained by subtracting the second weight from the first weight and subtracting the third total amount is used as a first difference, and the first difference is used as a weight value of free carbon in the transformer oil, based on a first preset volume of the transformer oil, a content of the weight of the free carbon in the transformer oil is obtained, that is, the obtained weight of the free carbon is divided by the first preset volume of the transformer oil measured in step 101, so as to obtain a content of the free carbon in the transformer oil, wherein a unit of the content of the free carbon is set to mg/ml.
In an embodiment, a second difference between the first weight and the second weight is calculated, the second difference is used as a weight value of a component in the transformer oil, and the content of the component is calculated based on the first preset volume of the transformer oil, that is, the obtained weight of the component is divided by the first preset volume of the transformer oil measured in step 101, so as to obtain the content of the component in the transformer oil, wherein the unit of the content of the component is set as mg/ml.
In one embodiment, since the last remaining solid powder material in the thermogravimetric analysis crucible is an inorganic component such as dust in the transformer oil, the third weight of the third solid powder material is taken as the weight value of the inorganic component in the transformer oil, and the content of the inorganic component is calculated based on the first preset volume of the transformer oil. And dividing the weight of the obtained inorganic component by the first preset volume of the transformer oil measured in the step 101 to obtain the content of the inorganic component in the transformer oil, wherein the unit of the content of the inorganic component is set as mg/ml.
In summary, the invention provides a method for measuring the free carbon content of transformer oil, which comprises the steps of mixing and shaking up a first preset volume of transformer oil and a second preset volume of petroleum ether to obtain a first mixed solution, and carrying out air release treatment on a centrifuge tube filled with the first mixed solution; centrifuging the centrifuge tube to separate supernatant liquid from the first mixed solution, taking the residual substances in the centrifuge tube as second mixed solution, and centrifuging the second mixed solution for preset times to obtain third mixed solution; adding petroleum ether with a third preset volume into the third mixed solution to obtain a fourth mixed solution, and carrying out ultrasonic treatment on a centrifugal tube filled with the fourth mixed solution; transferring the fourth mixed solution after ultrasonic treatment to a watch glass, carrying out air drying treatment on the fourth mixed solution in the watch glass to volatilize petroleum ether in the fourth mixed solution, drying the watch glass to obtain a first solid powder substance, and obtaining a first weight of the first solid powder substance; placing the first solid powder substance in a thermogravimetric analyzer so that the thermogravimetric analyzer conducts organic component cracking treatment on the first solid powder substance in a nitrogen flow mode to obtain a second solid powder substance, and obtaining a second weight of the second solid powder substance; enabling the thermogravimetric analyzer to perform combustion treatment on the second solid powder substance in an oxygen flow mode to obtain a third solid powder substance and obtain a third weight of the third solid powder substance; and calculating a first difference value between the second weight and the third weight, taking the first difference value as a weight value of free carbon in the transformer oil, and calculating the content of the free carbon based on the first preset volume of the transformer oil. Compared with the prior art, the technical scheme of the invention can improve the efficiency and accuracy of measuring the content of free carbon in the transformer oil, and the measuring process of the content of the free carbon is simple and the operation is convenient.
The above description is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and substitutions can be made without departing from the technical principle of the present invention, and these modifications and substitutions should also be regarded as the protection scope of the present invention.

Claims (10)

1. A method for measuring the free carbon content of transformer oil is characterized by comprising the following steps:
mixing and shaking up transformer oil with a first preset volume and petroleum ether with a second preset volume to obtain a first mixed solution, and degassing a centrifuge tube filled with the first mixed solution;
centrifuging the centrifuge tube to separate supernatant liquid from the first mixed solution, taking the residual substances in the centrifuge tube as second mixed solution, and centrifuging the second mixed solution for preset times to obtain third mixed solution;
adding petroleum ether with a third preset volume into the third mixed solution to obtain a fourth mixed solution, and carrying out ultrasonic treatment on the centrifuge tube filled with the fourth mixed solution;
transferring the fourth mixed solution after ultrasonic treatment to a watch glass, performing air drying treatment on the fourth mixed solution in the watch glass to volatilize petroleum ether in the fourth mixed solution, and drying the watch glass to obtain a first solid powder substance and obtain a first weight of the first solid powder substance;
placing the first solid powder substance in a thermogravimetric analyzer so that the thermogravimetric analyzer conducts organic component cracking treatment on the first solid powder substance in a nitrogen flow mode to obtain a second solid powder substance, and obtaining a second weight of the second solid powder substance; enabling the thermogravimetric analyzer to perform combustion treatment on the second solid powder substance in an oxygen flow mode to obtain a third solid powder substance and obtain a third weight of the third solid powder substance;
and calculating a first difference value between the second weight and the third weight, taking the first difference value as a weight value of free carbon in the transformer oil, and calculating the content of the free carbon based on the first preset volume of the transformer oil.
2. The method of claim 1, wherein obtaining a second weight of the solid powder material after combustion further comprises:
calculating a second difference value between the first weight and the second weight, taking the second difference value as a weight value of the component in the transformer oil, and calculating the content of the component based on the first preset volume of the transformer oil;
taking the third weight of the third solid powder substance as the weight of the inorganic components in the transformer oil, and calculating the content of the inorganic components based on the first preset volume of the transformer oil.
3. The method for measuring the free carbon content of the transformer oil according to claim 1, wherein the centrifuging process is performed on the second mixed solution for a preset number of times to obtain a third mixed solution, and specifically comprises the following steps:
obtaining petroleum ether with a second preset volume, mixing and shaking the petroleum ether with the second preset volume and the second mixed solution to obtain a fifth mixed solution, and carrying out air release treatment on a centrifuge tube filled with the fifth mixed solution;
centrifuging the centrifuge tube filled with the fifth mixed solution to separate supernatant from the fifth mixed solution, taking the residual substances in the centrifuge tube as a sixth mixed solution,
obtaining petroleum ether with a second preset volume again, mixing and shaking the petroleum ether with the second preset volume and the sixth mixed solution to obtain a seventh mixed solution, and carrying out air release treatment on the centrifuge tube filled with the seventh mixed solution;
and centrifuging the centrifuge tube filled with the seventh mixed solution to separate supernatant liquid from the seventh mixed solution, and taking the residual substances in the centrifuge tube as a third mixed solution.
4. The method for measuring the content of free carbon in transformer oil according to claim 1, wherein after the fourth mixed solution is transferred to a watch glass after ultrasonic treatment, the method further comprises:
the petroleum ether of the fourth preset volume is obtained, the petroleum ether of the fourth preset volume is added into a centrifugal tube filled with a fourth mixed liquid, so that the petroleum ether of the fourth preset volume is right for cleaning the centrifugal tube, and after cleaning, all substances in the centrifugal tube are transferred to a watch glass, wherein the value range of the fourth preset volume is 1-3 ml.
5. The method for measuring the free carbon content of the transformer oil as claimed in claim 1, wherein the petroleum ether is n-hexane.
6. The method for measuring the free carbon content of the transformer oil according to claim 1, wherein the first preset volume is 5-25 ml, the second preset volume is 5-25 ml, and the volume ratio of the first preset volume to the second preset volume is 1: 1-1: 5;
the value range of the third preset volume is 1-3 ml.
7. The method for measuring the free carbon content of the transformer oil according to claim 1, wherein the parameter setting of the thermogravimetric analyzer in the nitrogen flow mode comprises: setting the value range of nitrogen flow to be 30-50 ml/min, setting the value range of heating rate to be 10-20K/min, setting the value range of heating amplitude to be 40 +/-10 ℃ to 500 +/-50 ℃, and setting the value range of constant temperature time to be 500 +/-50 ℃ for 5-10 minutes.
8. The method for measuring the free carbon content of the transformer oil according to claim 1, wherein the parameter setting of the thermogravimetric analyzer in the oxygen flow mode comprises: setting the value range of oxygen flow to be 30-50 ml/min, setting the value range of temperature rise rate to be 10-20K/min, and setting the value range of temperature rise amplitude to be 500 +/-50 ℃ to 700 +/-50 ℃.
9. The method for measuring the free carbon content of the transformer oil according to claim 1, wherein a centrifugal tube filled with the third mixed solution is subjected to ultrasonic treatment, and the set ultrasonic time is within a range of 1-3 minutes.
10. The method for measuring the free carbon content of the transformer oil according to claim 1, wherein the watch glass is dried, and the drying temperature is set to be in a range of 40-60 ℃.
CN202210644856.7A 2022-06-08 2022-06-08 Method for measuring free carbon content of transformer oil Pending CN115032112A (en)

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CN115683932A (en) * 2023-01-05 2023-02-03 北京联合荣大工程材料股份有限公司 Method for measuring contents of C and SiC in commercial silicon carbide

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115683932A (en) * 2023-01-05 2023-02-03 北京联合荣大工程材料股份有限公司 Method for measuring contents of C and SiC in commercial silicon carbide

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