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Qualitative and quantitative analytic method of multiple sulfides in transformer oil

A transformer oil, quantitative analysis technology, applied in the direction of analysis materials, instruments, measuring devices, etc., can solve the problem that the quantitative detection method of multiple sulfides in oil is not yet clear, the types of corrosive sulfur in insulating oil cannot be given, and the qualitative detection is not accurate Sexuality and persuasiveness and other issues, to achieve the effect of strong practical application significance, convenient operation and wide application range

Inactive Publication Date: 2015-12-09
NORTH CHINA ELECTRIC POWER UNIV (BAODING)
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  • Abstract
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AI Technical Summary

Problems solved by technology

[0003] At present, the methods for detecting corrosive sulfur in transformer oil are all qualitative methods based on experience. By observing the color change of the copper sheet after the reaction to judge whether the oil sample is corrosive, these methods rely on the subjective perception and judgment of the color, and Only suitable for mineral oil without metal inhibitor additives, lacks accuracy and convincing for qualitative detection, and cannot give the type of corrosive sulfur in insulating oil
The determination methods of total sulfur content in transformer oil mainly include electrometry, ultraviolet fluorescence method, energy dispersive X-ray fluorescence spectrometry, high-temperature furnace combustion method, etc., but still cannot qualitatively analyze the types of sulfides in oil samples
The currently used qualitative detection methods for sulfides in oil have shortcomings such as low accuracy and difficulty in distinguishing sulfide types, and the quantitative detection method for multiple sulfides in oil has not yet been clarified.

Method used

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  • Qualitative and quantitative analytic method of multiple sulfides in transformer oil
  • Qualitative and quantitative analytic method of multiple sulfides in transformer oil
  • Qualitative and quantitative analytic method of multiple sulfides in transformer oil

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0047] Embodiment 1: determine various sulfide retention times

[0048]1) Sample preparation: add a certain concentration (1-1000ppm) of a single sulfur compound to be detected to unused transformer oil, and mix well to obtain oil samples containing different types of sulfides.

[0049] 2) Sampling: Use 2mL chromatographic headspace bottles to sample 1mL of oil samples containing different types of sulfides and unused transformer oil respectively, and seal them. Oil samples containing different types of sulfides were used as the experimental group, and unused transformer oil was used as the control group.

[0050] 3) GC-SCD detection: Set up the equipment according to the detection conditions given in Attached Table 1, place the experimental group and the control group on the quantitative (1uL) injector of the chromatograph for GC-SCD detection, and obtain the responses of the two Atlas.

[0051] 4) Determine the retention time: compare the corresponding spectra of each expe...

Embodiment 2

[0052] Example 2: Determining Response Factors

[0053] 1) Preparation of standard oil samples: Add 15 groups of dodecanethiol with different concentrations (1-1000ppm) to the transformer oil without dodecanethiol to make standard oil samples, and mix well.

[0054] 2) GC-SCD detection: Use 2mL chromatographic headspace vials to take 1mL of standard oil samples of different concentrations and seal them, then perform quantitative injection of 1uL for GC-SCD detection, and obtain the response spectrum of the standard oil samples.

[0055] 3) Determining the response factor: Integrate the response peaks that appear in the response spectrum (combining automatic and manual integration) to obtain the dodecanethiol response abundance (S) of standard oil samples with different concentrations, and then add the The molar concentration (mol / L) of elemental sulfur in dodecanethiol and the corresponding response abundance are plotted on the abscissa and ordinate, and the slope of the obtai...

Embodiment 3

[0056] Embodiment 3: sample qualitative and quantitative analysis

[0057] 1) Qualitative analysis of sulfide in the sample

[0058] Take 1mL of the sample with a 2mL chromatographic headspace bottle and seal it, carry out the GC-SCD detection of quantitative injection 1uL, obtain the response spectrum, according to the sulfide retention time determined in Example 1, qualitatively analyze the content of sulfide contained in the sample type.

[0059] 2) Quantitative analysis of sulfide in the sample

[0060] The GC-SCD detection spectrum of the sample in Example 1 is integrated (combined automatically with manual integration) to obtain the response abundance of each sulfide, and calculate the mass concentration of each sulfide in the sample to be analyzed according to formula (a) ( mg / kg).

[0061]

[0062] In the formula: X is the mass concentration of sulfide in the sample, mg / kg;

[0063] N is the number of sulfur atoms contained in the molecular formula of sulfide; ...

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Abstract

The invention belongs to the technical field of detection ofsulfides, and relates to a qualitative and quantitative analytic method of multiple sulfides in transformer oil on the basis of GC-SCD. The method includes determination of sulfide retention time, determination of response factors, and qualitative analysis and quantitative analysis of the sulfides in the sample. The method is used in detection of corrosive sulfur in non-used and operated mineral insulating oil, can determine the type and content of the corrosive sulfur in the oil more directly and accurately, and can be used for mastering potential threaten degree of the oil quality to a transformer better. The method is wide in adaptable range, is high in sensitivity, is wide in linear scope, is convenient to carry out, is accurate in result, is free of interference of non-sulfur compounds in the sample and has excellent practical application significance.

Description

technical field [0001] The invention belongs to the technical field of sulfide detection, and in particular relates to a qualitative and quantitative analysis method for multiple sulfides in transformer oil. Background technique [0002] At present, the transformer oil used in the power industry contains sulfur, nitrogen, oxygen and other elements in addition to a large amount of hydrocarbons. Sulfur mainly exists in the form of mercaptans, sulfides, sulfides, thiophenes and other compounds. closely related to the origin of crude oil. In the past ten years, hundreds of transformer failures have occurred worldwide due to corrosive sulfur in insulating oil, which has caused great harm to the safe and stable operation of the power grid. The accurate qualitative and quantitative analysis of corrosive sulfur in transformer oil has important practical significance for the prevention of transformer failure, state monitoring and life evaluation. [0003] At present, the methods fo...

Claims

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Application Information

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IPC IPC(8): G01N30/02
Inventor 周勇李庆民李方青
Owner NORTH CHINA ELECTRIC POWER UNIV (BAODING)