Iridium complex electrochemiluminescence kit for determining trace water in organic solvent

A chemiluminescence reagent and organic solvent technology, applied in the field of electrochemiluminescence kit development, can solve the problems of complex determination process, cumbersome reagent preparation, harsh preparation conditions, etc.

Inactive Publication Date: 2012-10-03
JIANGNAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the detection range of this standard method is very wide (ppm to 5%), it has advantages such as good repeatability and accuracy, but it still has many limiting shortcomings: reagent preparation is loaded down with trivial details; Preparation condition is harsh; Assay process is complicated; Toxic substances such as sulfur dioxide and pyridine will damage the health of operators, etc.
However, the use of electrochemiluminescence to measure trace water in organic solvents has not been reported yet.

Method used

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  • Iridium complex electrochemiluminescence kit for determining trace water in organic solvent
  • Iridium complex electrochemiluminescence kit for determining trace water in organic solvent
  • Iridium complex electrochemiluminescence kit for determining trace water in organic solvent

Examples

Experimental program
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Effect test

example 1

[0015] Example 1, the glassy carbon electrode is made of Al with a diameter of 0.05 μm 2 o 3 The suspension was polished on suede, then ultrasonically cleaned in absolute ethanol and ultrapure water for 1 min each, and dried in the air. Prepare a series of 3mL acetonitrile standard solutions with different water contents, the water contents from low to high are (v / v): 0.00%, 0.01%, 0.02%, 0.04%, 0.06%, 0.08%, 0.10%, 0.12%. Then completely dissolve the substances in the iridium complex electrochemiluminescence kit respectively, connect the three-electrode system to the electrochemiluminescence instrument, and measure the ECL intensity (see attached figure 2 ), with the water content as the abscissa and the ECL intensity as the ordinate to draw the working curve (see attached image 3 ). Measure the water content in the actual acetonitrile sample solvent, and find out from the working curve that the water content in the acetonitrile sample solvent is 0.023%.

example 2

[0016] Example 2, the glassy carbon electrode is made of Al with a diameter of 0.05 μm 2 o 3 The suspension was polished on suede, then ultrasonically cleaned in absolute ethanol and ultrapure water for 1 min each, and dried in the air. Prepare a series of 3mL DMF standard solutions with different water contents, the water contents from low to high are (v / v): 0.00%, 0.01%, 0.02%, 0.04%, 0.06%, 0.08%, 0.10%, 0.12%. Then completely dissolve the substances in the iridium complex electrochemiluminescence kit respectively, connect the three-electrode system to the electrochemiluminescence instrument, measure the ECL intensity, take the water content as the abscissa, and the ECL intensity as the ordinate to draw a working curve (see the appendix Figure 4 ). Measure the water content in the actual DMF sample solvent, and find out from the working curve that the water content in the DMF sample solvent is 0.064%.

example 3

[0017] Example 3, the glassy carbon electrode is made of Al with a diameter of 0.05 μm 2 o 3 The suspension was polished on suede, then ultrasonically cleaned in absolute ethanol and ultrapure water for 1 min each, and dried in the air. Prepare a series of 3 mL dichloromethane standard solutions with different water contents, the water contents from low to high are (v / v): 0.00%, 0.01%, 0.02%, 0.04%, 0.06%, 0.08%, 0.10%, 0.12 %. Then completely dissolve the substances in the iridium complex electrochemiluminescence kit respectively, connect the three-electrode system to the electrochemiluminescence instrument, measure the ECL intensity, take the water content as the abscissa, and the ECL intensity as the ordinate to draw a working curve (see the appendix Figure 5 ). Measure the water content in the actual dichloromethane sample solvent, and find out from the working curve that the water content in the dichloromethane sample solvent is 0.047%.

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Abstract

The invention belongs to development of an electrochemiluminescence kit which is used for sensitively and quickly determining trace water in an organic solvent. The kit comprises an efficient light-emitting substance, namely iridium complex, and supports electrolytes of tetrabutyl-ammonium hexafluorophosphate and sodium hydroxide. By the kit, the substance in the kit is required to be dissolved in a certain amount of the organic solvent, and the water content in the organic solvent can be measured by measuring the electrochemiluminescence intensity. The iridium complex electrochemiluminescence kit has the characteristics of high sensitivity, quick response, economical efficiency, practicability and particularly low detection limit.

Description

technical field [0001] The invention relates to the development of an electrochemiluminescence kit for detecting water content in organic solvents, and relates to the detection of trace amounts of water in common organic solvents such as acetonitrile, DMF, dichloromethane, acetone, benzene and toluene in application. Background technique [0002] The amount of water in an organic solvent is an important indicator of the quality of the organic solvent and an important factor affecting its performance. For example, the water content in the organic solvent affects the chemical reaction to a great extent, and the water in the organic solvent will also affect the sensitivity and accuracy of the determination in the analysis and detection, so the determination and control of the water content in the organic solvent is in the important in many applications. [0003] The standard method for water content analysis and determination is Karl Fischer titration, which is suitable for th...

Claims

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Application Information

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IPC IPC(8): G01N21/76G01N27/26
Inventor 宋启军朱胜男李春阳韩超峰
Owner JIANGNAN UNIV
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