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A method for the determination of furfural content in transformer oil by high performance liquid chromatography

A high performance liquid chromatography and transformer oil technology, applied in the field of transformers, can solve the problems of inability to extract furfural and low accuracy of furfural detection, and achieve the effects of simple implementation, shortening manpower and time costs, and significant social and economic benefits

Active Publication Date: 2019-11-19
ELECTRIC POWER RESEARCH INSTITUTE OF STATE GRID SHANDONG ELECTRIC POWER COMPANY +1
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] At present, the main method for detecting the content of furfural in transformer oil is to use methanol to extract furfural in the oil, and then use high performance liquid chromatography to measure it. However, this method has the following problems: although furfural has good selectivity in transformer oil, it can be extracted from transformer The oil is extracted into methanol, but the extraction rate is only about 70%, and the furfural in the transformer oil cannot be extracted completely, resulting in a relatively low detection accuracy of furfural in the transformer oil

Method used

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  • A method for the determination of furfural content in transformer oil by high performance liquid chromatography
  • A method for the determination of furfural content in transformer oil by high performance liquid chromatography
  • A method for the determination of furfural content in transformer oil by high performance liquid chromatography

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Effect test

Embodiment 1

[0070] Example 1 Exploration of chromatographic conditions

[0071] 1. The choice of mobile phase

[0072] (1) Select a phenylpropyl bonded silica gel column (5μm, Φ4.6×150mm);

[0073] Sample: The ethanol solution of oxidized furoic acid is used, and potassium permanganate is used for oxidation. Refer to Example 2.

[0074] Choose the following mobile phases when exploring, the following are just typical examples:

[0075] The volume ratio of methanol: water = 30: 70, chromatographic behavior: no chromatographic peak tailing phenomenon, but the column efficiency is poor;

[0076] Acetonitrile: water volume ratio = 30: 70, chromatographic behavior: chromatographic peak tailing;

[0077] The volume ratio of methanol:0.05mol / L sodium acetate aqueous solution=30:70, chromatographic behavior: chromatographic peaks appear bifurcated;

[0078] Methanol: 0.05mol / L sodium citrate (monosodium citrate, pH4.5) aqueous solution volume ratio=30:70, chromatographic behavior: chromatographic peak shape a...

Embodiment 2

[0118] Choice of oxidation method:

[0119] Before determining the oxidation method most suitable for the present invention, the present invention has been studied and explored through various oxidation methods. Among them, experiments have verified that the Conicano method produces a large amount of other by-products while preparing furoic acid, which increases the difficulty of chromatographic separation; the oxidation efficiency of the catalyst oxidation method is low, and it cannot completely oxidize furfural. Furoic acid, which is not conducive to the detection of furoic acid. Using the oxidant oxidation method, the present invention first found that in transformer oil containing furfural in a certain concentration range (between 5.2μg / L~5mg / L), the transformer oil is oxidized by the oxidant method, and the furoic acid reaction yield is certain Yes, and the present invention adopts oxidant oxidation method, which has higher yield and fewer by-products.

[0120] Take the pref...

Embodiment 3

[0124] (1) Selection of extractant types:

[0125] Select methanol, ethanol, water, methanol: water volume ratio of 1:1, ethanol and water volume ratio of 1:1 as extractants.

[0126] experimental method:

[0127] Dissolve 0.010g furoic acid and 0.010g furfural in 10ml blank transformer oil and mix them thoroughly; then select the above 5 extractants for extraction, the pH of the extractant is 6.5, and the volume ratio of extractant: blank transformer oil is 10 : 3. During extraction, vibrate the sample on a mechanical vibrator for 5 minutes and let the sample stand until the extraction phase and the oil phase are completely separated.

[0128] The experimental results are shown in the table. From Table 4, the extraction efficiency of furoic acid and furfural is different for different extractants. Among them, when ethanol is used as the extractant, furoic acid has the highest extraction efficiency, while furfural has the lowest extraction efficiency.

[0129] Table 4 The extraction r...

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Abstract

The invention discloses a method used for measuring content of furfural in transformer oil via high performance liquid chromatography. The method comprises following steps: 1, pretreatment of transformer oil, wherein oxidation of the transformer oil with an oxidizing agent is carried out, after oxidation, ethanol is taken as an extraction agent for extraction so as to obtain an extracted solution 1, and ethanol is also taken as an extraction agent to extract the untreated transformer oil so as to obtain an extracted solution 2; and 2, yield measurement of oxidation of the transformer oil into furfural, wherein the oxidation method and the oxidation conditions in the step 1 are adopted, and the reaction yield of oxidation of furfural in the transformer oil into furoic acid is carried out; 3, high performance liquid chromatography measurement, wherein a phenylpropyl bonded silica gel chromatographic column is adopted, a sodium citrate aqueous solution and methanol are taken as the mobile phase, wherein the pH value of the sodium citrate aqueous solution is controlled to be 4 to 5; and 4, measurement of furfural content. The method can be used for measuring furfural in transformer oil accurately.

Description

Technical field [0001] The invention belongs to the technical field of transformers, and specifically relates to a method for determining the furfural content of transformer oil by high-performance liquid chromatography. Background technique [0002] Transformer oil refers to a type of insulating oil used in oil-filled electrical equipment such as transformers for insulation, cooling and arc extinguishing. In oil-filled electrical equipment, the aging of the fibrous material that constitutes the solid insulation leads to the decomposition of cellulose to produce several compounds, such as furfural and furan derivatives. Most of the furan derivatives are adsorbed on paper, while a small part is dissolved. In the oil. The presence of these substances can be used as a diagnostic basis for the aging of the solid insulation of operating equipment, and can also be used as a supplement to the analysis of dissolved gases. [0003] At present, the main methods for detecting furfural in tr...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/06G01N30/74
CPCG01N30/06G01N30/74
Inventor 陈素红高峰韩志骏于乃海许乃媛
Owner ELECTRIC POWER RESEARCH INSTITUTE OF STATE GRID SHANDONG ELECTRIC POWER COMPANY
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