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Method for rapidly detecting content of antioxidant in transformer insulating oil

A technology for transformer insulating oil and antioxidants, which is used in measuring devices, instruments, scientific instruments, etc., can solve the problems of decolorization, complex color rendering processing, human health and environmental hazards, and measurement errors, etc., and achieve high sensitivity and high-efficiency detection. , the effect of easy operation

Pending Publication Date: 2022-02-08
ELECTRIC POWER RES INST OF STATE GRID ANHUI ELECTRIC POWER +2
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Among them, spectrophotometry has the advantages of low requirements for instruments and strong versatility, but the decolorization and color development in the process of sample processing are relatively complicated, and there are errors in the measurement of samples that become darker after aging; infrared spectroscopy has the advantage of not requiring sample processing. , the advantage of fast analysis speed, but the requirements for the instrument are relatively high, and the potassium bromide liquid pool used is prone to equipment failure due to damp and other reasons; liquid chromatography requires a liquid chromatograph, which has the advantages of high test accuracy, For example, in the patent with publication number CN104007192A, high performance liquid chromatography is used to measure antioxidants in insulating oil, but a large amount of methanol mobile phase is required in the measurement process, and a large amount of waste liquid is generated after the test, which is harmful to human health and the environment

Method used

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  • Method for rapidly detecting content of antioxidant in transformer insulating oil
  • Method for rapidly detecting content of antioxidant in transformer insulating oil
  • Method for rapidly detecting content of antioxidant in transformer insulating oil

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] (1) Preparation of antioxidant BHT standard solution

[0039] Accurately weigh 0.20g of the standard substance BHT, add 20ml of chromatographically pure methanol, and prepare a standard solution mother solution with a concentration of 10mg / ml; use the standard mother solution to prepare 1.0mg / ml, 0.2mg / ml, 0.1mg / ml, 0.075 mg / ml, 0.05mg / ml, 0.025mg / ml, 0.01mg / ml, 0.005mg / ml, 0.001mg / ml, 0.0001mg / ml BHT solution.

[0040] (2) Drawing of standard working curve

[0041] Select the fluorescence spectrophotometer (HITACHI F-7100FL Spectrophotometer) condition of the present invention, i.e. excitation start wavelength: 220.0nm, excitation cut-off wavelength: 420.0nm, emission start wavelength: 240.0nm, emission cut-off wavelength: 520.0nm, scanning speed : 2400nm / min, photomultiplier tube voltage: 400V, excitation scanning slit width: 5.0nm, emission scanning slit width 5.0nm.

[0042] Take antioxidant BHT standard solution to measure three-dimensional fluorescence. The measu...

Embodiment 2

[0045] Determination of the actual sample to be tested

[0046] Accurately weigh 0.20g of the standard substance BHT, add blank oil to 20g, and prepare a calibration solution mother solution with a concentration of 1% (mass fraction); weigh 3.00g of the calibration solution mother solution in a 50mL centrifuge tube, and then add 7.00g of blank oil sample (At this time, the BHT content is 0.3% (mass fraction)), add 5 mL of methanol, plug the tube tightly, place it horizontally on a mechanical shaker at room temperature for 15 minutes, and then centrifuge in a high-speed centrifuge until the two phases of methanol and oil are completely separated ( Rotational speed is 5000rpm, time is 5min), take out 3mL supernatant liquid with syringe, after diluting 100 times, measure three-dimensional fluorescence, substitute into the standard curve to calculate the content of actual BHT.

[0047] The test results of the actual sample of antioxidant BHT are as follows: Figure 4 and shown in...

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Abstract

The invention discloses a method for rapidly detecting the content of an antioxidant in transformer insulating oil, and belongs to the technical field of power system device transformer insulation state evaluation. The method comprises the following steps of: (1) preparing a series of antioxidant standard solutions with concentration gradients by adopting chromatographically pure-grade methanol, measuring three-dimensional fluorescence, and drawing an antioxidant standard curveby taking the concentrations of the antioxidants as the abscissa and the fluorescence intensity of the antioxidant as the ordinate; and (2) extracting an antioxidant in transformer insulating oil into methanol, measuring three-dimensional fluorescence, and substituting the three-dimensional fluorescence into the standard curve in the step (1) to obtain the content of 2, 6-di-tert-butyl p-cresol. The method has the advantages of simple and convenient operation, high sensitivity, small sample use amount and high analysis efficiency, and can effectively avoid the harm to human health and environment caused by a large amount of waste liquid generated after a liquid chromatography test; the method not only is simple in sample treatment, but also can rapidly and accurately calculate the content of the antioxidant BHT in the transformer oil.

Description

technical field [0001] The invention relates to the technical field of evaluating the insulation state of a transformer in a power system device, in particular to a method for rapidly detecting the antioxidant content in transformer insulating oil. Background technique [0002] Transformer oil occupies a high proportion in power equipment, and its aging problem is a key factor related to the safe operation of the power grid. With the prolongation of operation time, the transformer oil will be oxidized, aged and other phenomena will be generated, such as aldehydes, ketones, acids, esters and sludge, etc., will be formed, which will seriously affect the insulation performance of transformer oil. The rapid development of the power grid puts forward high requirements for the assessment of the aging state of transformers. Adding antioxidants to transformer oil is an effective way to delay the oxidation rate of oil products. Since insulating oil contains rich aging information, ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N21/64
CPCG01N21/643
Inventor 赵跃宋玉梅马凤翔徐芳朱峰刘子恩谢佳赵恒阳袁小芳冷威李坤鹏
Owner ELECTRIC POWER RES INST OF STATE GRID ANHUI ELECTRIC POWER
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