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Pretreatment method for measuring passivator in transformer oil

A transformer oil and passivating agent technology, applied in the preparation of test samples, etc., can solve the problems of difficult to overcome sample matrix interference and low extraction efficiency

Inactive Publication Date: 2012-02-01
EAST CHINA ELECTRIC POWER TEST & RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Most of the original conventional methods separate the analyte from the interfering substances by selecting a suitable organic solvent for liquid-liquid extraction, which has the disadvantages of low extraction efficiency and difficulty in overcoming the interference of the sample matrix.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0010] Weigh 2 grams of transformer oil and dissolve it in 5 milliliters of n-pentane, pass through the solid-liquid extraction column, and after the activation equilibrium of 2 milliliters of n-pentane, gradually load the sample on the solid-liquid extraction column at a flow rate of 3 ml / min, successively Rinse with 10 ml of n-pentane twice, dry in vacuum for 10 minutes, enrich the analytes on the solid-liquid extraction column; then elute with 70:30 methanol aqueous solution, collect into a volumetric flask and carry out fixed To complete the pretreatment of the sample.

Embodiment 2

[0012] Weigh 5 grams of transformer oil and dissolve it in 5 milliliters of n-pentane, pass through the solid-liquid extraction column, and after the activation equilibrium of 4 milliliters of n-pentane, gradually load the sample on the solid-liquid extraction column at a flow rate of 0.8 ml / min, successively Rinse with 10 ml of n-pentane twice, dry in vacuum for 8 minutes, enrich the analyte on the solid-liquid extraction column; then elute with 70:30 methanol water solution, collect it in a volumetric flask and carry out fixed To complete the pretreatment of the sample.

Embodiment 3

[0014] Weigh 1 gram of transformer oil and dissolve it in 5 ml of n-hexane, pass through the solid-liquid extraction column, and after the activation equilibrium of 4 ml of n-hexane, gradually load the sample onto the solid-liquid extraction column at a flow rate of 2.5 ml / min, twice successively Rinse with 10 ml of n-pentane respectively, and dry in vacuum for 8 minutes, so that the analyte is enriched on the solid-liquid extraction column; then eluted with methanol, collected into a volumetric flask and fixed to volume, and the pretreatment of the sample is completed. deal with.

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Abstract

The invention provides a pretreatment method for measuring a passivator in transformer oil. The method comprises the following steps of: weighing 1-5g of transformer oil, and dissolving in 5ml of n-pentane; activating and balancing in 2-4ml of activating agent by using a solid-liquid column extractor; gradually sampling to the solid-liquid column extractor with the flow rate of lower than 1-4ml / min; respectively washing twice by using 10ml of n-pentane; drying for 8-10min in vacuum to ensure that an object to be measured is enriched on the solid-liquid column extractor; eluting by using an eluant; collecting to a measuring bottle for measuring; and completing pretreatment of a sample. By using the method, a high-purity and concentrated target detecting object can be enriched, other interference impurities are removed, the quality is stable, and the sample has high recovery rate.

Description

technical field [0001] The invention relates to a pretreatment method for measuring passivating agent in transformer oil. Background technique [0002] Sample pretreatment is an indispensable key step in chemical analysis methods. The passivating agent is an oil-soluble substance, and the matrix of the sample of the passivating agent added to the transformer oil is mainly transformer oil. Transformer oil is a mixture of non-polar or weakly polar compounds such as long-chain alkanes, cycloalkanes and a small amount of aromatic hydrocarbons. The matrix components are complex and there are many interfering substances. Most of the original conventional methods separate the analyte from the interfering substances by selecting a suitable organic solvent for liquid-liquid extraction, which has the disadvantages of low extraction efficiency and difficulty in overcoming the interference of the sample matrix. Contents of the invention [0003] The technical problem to be solved by...

Claims

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Application Information

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IPC IPC(8): G01N1/28G01N1/34G01N1/40
Inventor 朱向群龚秋霖厉敏宪彭伟
Owner EAST CHINA ELECTRIC POWER TEST & RES INST