Fluorescent detection method of ion concentration in transformer oil

A technology of transformer oil and ion concentration, which is applied in chemical instruments and methods, fluorescence/phosphorescence, preparation of test samples, etc. Avoid operating steps and testing instruments, and have the effect of fast detection response and strong practicability

Active Publication Date: 2021-07-16
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, it is very difficult to detect ions directly in transformer oil.
On the one hand, transformer oil is a very poor solvent, and the particle size of metal-organic framework materials is at least tens to hundreds of nanometers, which is difficult to disperse uniformly in transformer oil, resulting in inaccurate test results
On the other hand, due to the autofluorescence of transformer oil, it will affect the effect of fluorescence detection
Therefore, no fluorescence detection method for ion concentration in transformer oil has been reported. It is of great significance to develop a method that can use the fluorescence of metal-organic framework materials to detect ion concentration in transformer oil.

Method used

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  • Fluorescent detection method of ion concentration in transformer oil
  • Fluorescent detection method of ion concentration in transformer oil
  • Fluorescent detection method of ion concentration in transformer oil

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Utilize the DMF solution of MOF-525 to detect the copper ion concentration in transformer oil by extraction method, and its concrete synthesis method is as follows:

[0028] Accurately weigh 1.35 g of benzoic acid and 105 mg of zirconium oxychloride, dissolve in 8 mL of DMF, and place the resulting solution in an oven at 80° C. to react for 2 hours. After cooling to room temperature, 47 mg of tetrakis(4-carboxyphenyl)porphyrin (TCPP) was dissolved by sonication. Next, the mixed solution was heated to 80° C. and reacted for 24 hours, cooled, centrifuged, and washed three times with DMF. After cleaning, 10 mL of DMF was added to the centrifuge tube, and 6000 mg / L MOF-525 solution was obtained after sonication. Subsequently, the above MOF-525 solution was diluted to 6 mg / L with DMF solvent to obtain a DMF solution of MOF-525 for detecting copper ions in transformer oil.

[0029] This solution was mixed with transformer oil containing different concentrations of copper io...

Embodiment 2

[0034] Utilize the aqueous solution of MOF-525 to detect the copper ion concentration in transformer oil by extraction method, and its specific synthetic route is as follows:

[0035]Accurately weigh 1.35g of benzoic acid and 105mg of zirconyl chloride, dissolve them in 8mL of DMF, and place the resulting solution in an oven at 80°C for 2 hours to react. After cooling to room temperature 47 mg tetrakis(4-carboxyphenyl)porphyrin (TCPP) was dissolved and sonicated. Next, the mixed solution was heated to 80° C. and reacted for 24 hours. After cooling, it was centrifuged and washed three times with deionized water. After cleaning, 10 mL of deionized water was added to the centrifuge tube, and a 6000 mg / L MOF-525 solution was obtained after ultrasonication. Subsequently, the above MOF-525 solution was diluted to 6 mg / L with deionized water to obtain an aqueous solution of MOF-525 for detecting copper ions in transformer oil.

[0036] Mix this solution with transformer oil contain...

Embodiment 3

[0039] Using the aqueous solution of R101@ZIF-67 to detect the concentration of iron ions in transformer oil by extraction method, the specific synthesis route is as follows:

[0040] Accurately weigh 0.1g of cobalt nitrate hexahydrate and dissolve it in 8mL of deionized water, add 300μL of an aqueous solution with a concentration of 1mg / mL rhodamine 101 and stir for 20 minutes, and accurately weigh 0.2g of 2-methylimidazole and dissolve it in 8mL of deionized water , the two solutions were mixed and stirred at room temperature for 6 h. After the reaction was completed, they were collected by centrifugation and washed three times with deionized water. After cleaning, take 6 mg of sample, add 10 mL of deionized water, and obtain a high-concentration R101@ZIF-67 aqueous solution after ultrasonication. Then the above R101@ZIF-67 solution was diluted to 6 mg / L with deionized water to obtain an aqueous solution of R101@ZIF-67 for detecting iron ions in transformer oil.

[0041] Mi...

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Abstract

The invention discloses a fluorescence detection method for the concentration of ions to be measured in transformer oil. The method is to extract the ions in the transformer oil into a detection reagent by using an extraction method, and realize the specific fluorescence response of the detection reagent to the ions in the oil. ion detection. The specific method is as follows: the metal-organic framework material capable of specific fluorescent detection of ions is mixed with a solvent to obtain a detection reagent, and after being fully mixed with the transformer oil to be tested, the change in the fluorescence intensity of the solution is tested, so as to realize the detection of the ions to be tested in the oil and detection of its content. The method is easy to operate, low in cost, accurate in measurement results, free from complex electromagnetic environment interference, and can effectively avoid the interference of oil autofluorescence and the problem that fluorescent materials are difficult to dissolve in oil, and has good practical application prospects.

Description

technical field [0001] The invention relates to an operation method for detecting ions in transformer oil, in particular to a method for detecting the concentration of ions to be measured in transformer oil by using a fluorescent metal-organic framework material solution. Background technique [0002] In the industrial field, the detection of ions in transformer oil is of great significance. The content of copper ions and iron ions in the insulating oil of transformers is an important basis for directly judging the aging of transformer insulation. When the copper and iron ions in the transformer oil are abnormally increased, it indicates that the insulation aging is accelerated and needs to be repaired in time. Although there is no latent fault in the transformer in operation, an analysis of the metal content in the oil should be done as the original data. After the transformer has a fault, the copper and iron ion content in the oil can be analyzed for comparison and fault ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N21/64G01N1/40C09K11/06C08G83/00
CPCC08G83/008C09K11/06C09K2211/1007C09K2211/1029C09K2211/1044C09K2211/1048C09K2211/1059C09K2211/182C09K2211/183C09K2211/187C09K2211/188G01N1/4055G01N21/643G01N2001/4061G01N2021/6432
Inventor 杨雨王迪张骏钱国栋崔元靖
Owner ZHEJIANG UNIV
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