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Method for determining content of potassium tert-butoxide

A technology of potassium tert-butoxide and content, which is used in material excitation analysis, fluorescence/phosphorescence, etc., can solve the problems of long time and complicated operation, and achieve the effect of simple operation, high sensitivity and high accuracy.

Inactive Publication Date: 2016-03-30
NANJING FORESTRY UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the main method for detecting the content of potassium tert-butoxide is acid-base titration, which is complicated to operate and takes a long time

Method used

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  • Method for determining content of potassium tert-butoxide
  • Method for determining content of potassium tert-butoxide
  • Method for determining content of potassium tert-butoxide

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Experimental program
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Effect test

Embodiment 1

[0019] The preparation of embodiment 1 salicylaldehyde azine

[0020] In a 250mL three-necked flask equipped with a thermometer, a stirrer and a reflux condenser, 2.44g (0.02mol) of salicylaldehyde, 100mL of absolute ethanol and 0.63g (0.01mol) of hydrazine hydrate were added successively, and heated to reflux for 2 hours. After cooling, a large amount of yellow precipitates were produced. Add 1mL of 30% hydrochloric acid, heat to dissolve and reflux for 2h, use the residual heat of the oil bath to cool slowly, and filter to obtain the crude product of needle-shaped yellow crystals. Put the crude product into a 250mL single-necked flask, add 200mL of absolute ethanol, heat and reflux in an oil bath for 2 hours, stop heating, and slowly cool down the reflux liquid using the residual temperature of the oil bath for recrystallization, and filter to obtain salicylaldehyde azine Yellow needle-like crystals, The yield was 89%.

[0021] The melting point of salicylaldehyde azine is ...

Embodiment 2

[0025] Embodiment 2 Potassium tert-butoxide is measured

[0026] Salicylaldehyde azine and potassium tert-butoxide were formulated into 13 kinds of ethanol solutions with different concentrations, wherein the concentration of salicylaldehyde azine was 1.0×10 -4 M, the concentration of potassium tert-butoxide is 0~32.0×10 -4 M. The fluorescence intensity changes of these 13 solutions were measured under the condition that the excitation wavelength was 385nm, as figure 2 shown. The results showed that potassium tert-butoxide had a good fluorescence enhancement effect on salicylaldehyde azine, which gradually increased with the concentration of potassium tert-butoxide.

[0027] When the concentration of potassium tert-butoxide is 0.5, 1.0, 1.5, 2.0, 2.5, 3.0, 3.5, 4.0×10 -4 M, the fluorescence intensity of these 8 systems increases linearly with the increase of concentration, and the linear relationship between fluorescence intensity and potassium tert-butoxide concentration...

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Abstract

The invention discloses a method for determining the content of potassium tert-butoxide. According to the method, salicylaldehyde azine is used as an organic fluorescent molecule for determining the content of potassium tert-butoxide. By applying the salicylaldehyde azine as the organic fluorescent molecule to the content determination of potassium tert-butoxide, the method has the advantages that the determination is convenient, the linearity is good, the sensitivity is high, the quality requirements are met, and RSD is relatively small and is 1.5%; salicylaldehyde and hydrazine hydrate are taken as reactants and are recrystallized to generate yellow salicylaldehyde azine acicular crystals. The method is a novel method for slowly cooling and crystallizing after hydrochloric acid is added for reflux and is simple, and the operation is easy.

Description

technical field [0001] The invention belongs to the technical field of fluorescence detection of potassium tert-butoxide, and in particular relates to a method for determining the content of potassium tert-butoxide. Background technique [0002] Potassium tert-butoxide is a non-nucleophilic strong base, the basicity is between potassium hydroxide and amino base, as an important catalyst, it is widely used in the condensation, heavy In reactions such as row and ring opening. However, the main method for detecting the content of potassium tert-butoxide is acid-base titration, which is complicated to operate and takes a long time. Therefore, the development and utilization of advanced instruments to determine the method of potassium tert-butoxide content has good practical value. [0003] Fluorescence spectroscopy has the advantages of rapid detection and high sensitivity. In recent years, the detection of metal ions and small organic molecules by fluorescence photometry has...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N21/64
CPCG01N21/64
Inventor 王石发杨金来徐徐杨益琴徐海军芮坚曹晓琴丁志斌王芸芸王忠龙杨丽娟谷文
Owner NANJING FORESTRY UNIV