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Reversed phase high performance liquid chromatography method for determining content of dibenzyl disulfide in insulating oil

A technology of dibenzyl disulfide and reverse high-efficiency liquid phase, which is applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problems of high cost and limited application, and achieve high repeatability, accuracy and simple operation , The effect of low price of equipment

Inactive Publication Date: 2016-09-28
HEILONGJIANG ELECTRIC POWER RES INST +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose of the present invention is to solve the problem of high cost and limited application of the existing gas chromatography-mass spectrometry method for measuring the content of DBDS in insulating oil, and provide a reverse high performance liquid chromatography for measuring the content of dibenzyl disulfide in insulating oil method

Method used

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  • Reversed phase high performance liquid chromatography method for determining content of dibenzyl disulfide in insulating oil

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specific Embodiment approach 1

[0021] Specific embodiment one: a kind of reverse high performance liquid chromatography method for measuring the content of dibenzyl disulfide in insulating oil according to the present embodiment is carried out according to the following steps:

[0022] 1. Preparation of stock solution: Weigh 0.100g of dibenzyl disulfide and 99.900g of blank oil, mix and stir at a temperature of 45-55°C until dibenzyl disulfide is completely dissolved, and then turn brown Store in a grinding bottle at a temperature of 3-5°C for later use;

[0023] If the stock solution is stored at a temperature of 3-5°C, the effective time is 3 months;

[0024] 2. Preparation of calibration solution: take five parts of the stock solution prepared in step 1, add blank oil to it and mix evenly, and prepare the concentrations as 5mg / kg, 50mg / kg, 100mg / kg, 300mg / kg and 500mg / kg calibration solution;

[0025] The valid time of the calibration solution shall not exceed 3 days;

[0026] 3. Preparation of solid-...

specific Embodiment approach 2

[0035] Specific embodiment 2: The difference between this embodiment and specific embodiment 1 is: after mixing in step 1, stir at a temperature of 48-53° C. until the dibenzyl disulfide is completely dissolved. Other steps and parameters are the same as those in the first embodiment.

specific Embodiment approach 3

[0036] Embodiment 3: This embodiment is different from Embodiment 1 or Embodiment 2 in that: in step 1, after mixing, stir at a temperature of 50° C. until dibenzyl disulfide is completely dissolved. Other steps and parameters are the same as those in Embodiment 1 or 2.

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Abstract

A reverse-phase high-performance liquid chromatography method for the determination of dibenzyl disulfide content in insulating oil. The invention relates to a method for measuring the content of dibenzyl disulfide in insulating oil. The purpose of the invention is to solve the problems of high cost and limited application of the existing gas chromatography-mass spectrometry method for determining the content of DBDS in insulating oil. Methods: 1. Preparation of stock solution; 2. Preparation of calibration solution; 3. Preparation of solid phase extraction adsorption column; 4. Preparation of sample solution; 5. Sample analysis; 6. Establishment of calibration curve; 7. Insulation to be tested Determination of dibenzyl disulfide content in oil. The method of the invention utilizes a relatively cheap liquid chromatograph to realize the determination of the dibenzyl disulfide content in the insulating oil, and the method is simple in operation, high in repeatability and accuracy, low in instrument equipment price, and easy to implement.

Description

technical field [0001] The invention relates to a method for measuring the content of dibenzyl disulfide in insulating oil. Background technique [0002] In recent years, transformer failures caused by corrosive sulfur in insulating oil have occurred frequently at home and abroad, which has brought great harm to the safety of the power grid and caused great economic losses and social impacts. Corrosive sulfur in insulating oil has high corrosion activity to metals, and can directly react with metals to form metal sulfides under certain conditions, causing corrosion damage to high-voltage electrical equipment materials, including elemental sulfur, hydrogen sulfide, mercaptan, Thioether, and some organic small molecule sulfides. The test results show that dibenzyl disulfide (DBDS) in insulating oil is the cause of Cu produced during transformer operation. 2 S and causes solid insulation breakdown, currently forming Cu 2 S transformer oil contains DBDS. The International El...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/89
CPCG01N30/89
Inventor 李国兴姜子秋付丽君李琳关艳玲
Owner HEILONGJIANG ELECTRIC POWER RES INST
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