Quantitative evaluation method for measuring corrosive sulfur by X-fluorescence

A corrosive sulfur, quantitative evaluation technology, applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problems of inaccurate qualitative analysis, increased technical difficulty, subjectivity, etc., to avoid misjudgment and reduce misjudgment of corrosiveness Sulfur, the effect of strong operational practicability

Inactive Publication Date: 2019-07-16
GUANGZHOU MECHANICAL ENG RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] 1) Judging the appearance color of copper materials is relatively subjective, and it is difficult to determine the complex and diverse surface colors, and it is easy to misjudge corrosiveness and non-corrosion
[0006] 2) When the surface of the copper material is judged to be non-corrosive, there may be a small amount of active sulfur, which cannot be reflected, resulting in corrosion of equipment
The color change on the surface of copper material is a quantitative change to a certain extent, which is meaningful for equipment failure, but it is difficult to determine the initial potential failure of the equipment
[0007] 3) When the sample has a lot of black suspended matter, a layer of black matter that cannot be cleaned will be adsorbed on the surface of the copper material, which will lead to misjudgment of the result, and

Method used

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  • Quantitative evaluation method for measuring corrosive sulfur by X-fluorescence
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  • Quantitative evaluation method for measuring corrosive sulfur by X-fluorescence

Examples

Experimental program
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Embodiment 1

[0042] A kind of quantitative evaluation method of measuring corrosive sulfur by X fluorescence of the present invention, described method comprises the following steps:

[0043] 1) Use a 100mL graduated cylinder to take 15mL uniform sample and put it into a 20mL headspace bottle;

[0044] 2) Polish the copper test piece samples a, sample b, sample c, sample d, sample e, and sample f with 240-mesh sandpaper respectively, and clean them with petroleum ether III, and use an X fluorescence sulfur meter to detect whether the copper test piece contains Sulfur, without sulfur, put the copper test piece into the container where the sample has been taken, ensure that the copper test piece is completely immersed in the oil, and cover the metal cover with rubber gasket;

[0045] 3) Open the oven in advance, set the temperature at 150±3°C, and keep the temperature constant for more than 30 minutes, put the above container in the oven at 150°C±3°C, keep the temperature constant for 24h or...

Embodiment 2

[0053] The precision (repeatability) of embodiment 2 method

[0054] In the same experiment, the same test product is carried out according to the method of embodiment 1 by the same experimenter, and the experiment is repeated at least 6 times to investigate the repeatability of the method. The results are as shown in table 2:

[0055] Table 2

[0056]

[0057] As can be seen from Table 2, the precision of the X fluorescence test corrosive sulfur quantitative analysis method of the copper test piece of the present invention is 13.8%, as seen this method precision is high, and repeatability is good.

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Abstract

The invention discloses a quantitative evaluation method for measuring corrosive sulfur by X-fluorescence. The quantitative evaluation method for measuring corrosive sulfur by the X-fluorescence comprises the following steps that (1) a sample is placed into a container; (2) a sulfur-free copper test piece is placed into the container with the sample taken out, it is ensured that the copper test piece is completely immersed into oil, and the container is sealed; (3) the container containing the cooper test piece in the step (2) is placed into an oven with the temperature of 150 DEG C+/-3 DEG C,constant temperature is carried out for 24-72h, and the container is taken out after an experiment is completed; (4) the sample is poured out after heating is completed, the cooper test piece is taken out and immersed into a cleaning solvent, and the attached sample on the cooper test piece is cleaned; (5) sulfur content test is carried out on the cooper test piece by using the X-fluorescence; and (6) a result is judged. According to the quantitative evaluation method for measuring corrosive sulfur by the X-fluorescence, after cooper, sulfur and a compound generate chemical reaction through the experiment, the condition of cooper test piece sulfur-containing compound is tested through X-fluorescence to judge whether an active sulfur compound exists in the oil or not, the quantitative evaluation method for measuring corrosive sulfur by the X-fluorescence can accurately judge the condition of corrosive sulfur and non-corrosive sulfur, and the operation practicability is high.

Description

technical field [0001] The invention relates to the technical field of transformer oil corrosive sulfur detection, in particular to a quantitative evaluation method for measuring corrosive sulfur by X-ray fluorescence. Background technique [0002] At present, the corrosive sulfur detection methods of electric power oil (mainly referring to transformer oil) include: SH / T 0304, SH / T 0804, GB / T 25961, DL / T 285, etc. The basic principles are based on different conditions and different specifications The copper material reacts with the sulfide in the electrical insulating oil. After passing the test, the appearance of the copper material, if the surface shows any one of graphite gray, dark brown or black, it is judged as corrosive sulfur, and other colors are non-corrosive. corrosion. [0003] Sulfur is one of the constituent elements of petroleum. It exists in crude oil in the form of elemental sulfur, hydrogen sulfide, and organic sulfides such as mercaptan, sulfide, disulfid...

Claims

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Application Information

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IPC IPC(8): G01N23/223
CPCG01N23/223
Inventor 贺石中王永安张文庞晋山张琳颖丘晖饶张驰吕清君梁幸李智婷
Owner GUANGZHOU MECHANICAL ENG RES INST
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