Quantitative evaluation method for measuring corrosive sulfur by X-fluorescence

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...

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 the generation of black matter such as copper oxide will also easily lead to misjudgment of the result

[0008] The existing Chinese patent 201510434614.5 discloses a qualitative and quantitative analysis method for multiple sulfides in transformer oil, which uses the advantages of a sulfur chemiluminescence detector and a gas chromatograph to analyze the possible sulfides in transformer oil. , is to analyze by detecting the types and contents of corrosive sulfur compounds, but there are many kinds of corrosive sulfur compounds, which need to be detected and determined one by one, and the technical difficulty increases. One-to-one correspondence between compounds), if the detection cannot cover all corrosive sulfur compounds, there will be missed detection of corrosive sulfur compounds, resulting in inaccurate qualitative analysis

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