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Method for measuring content of triethylamine in solvent containing trace water by ultraviolet spectroscopy

A technology of ultraviolet spectroscopy and triethylamine, which is applied in the direction of color/spectral characteristic measurement, measuring device, and material analysis through optical means, which can solve the problems of unsatisfactory and low timeliness, and achieve high timeliness and accurate detection results Reliable, easy-to-operate results

Pending Publication Date: 2022-05-17
甘肃银光聚银化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, although these methods can effectively measure low-content triethylamine, their timeliness is not high and cannot meet the needs of actual production.

Method used

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  • Method for measuring content of triethylamine in solvent containing trace water by ultraviolet spectroscopy
  • Method for measuring content of triethylamine in solvent containing trace water by ultraviolet spectroscopy

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Embodiment 1: the mensuration of triethylamine in acidic water, solvent is dichloromethane.

[0019] Determination of the density of triethylamine and dichloromethane. Since the organic components in the sample are easy to volatilize, pipetting the solution by volume is convenient for operation and helps to reduce experimental errors.

[0020] First, dichloromethane is added to the acidic water, the pH value is adjusted to strong alkalinity for extraction, the lower layer of dichloromethane layer is taken as the solution to be tested, and the density of the solution to be tested is measured. Prepare 10ml of dichloromethane-triethylamine stock solution, the theoretical content of triethylamine in the stock solution is 10‰. Take three parts of the solution to be tested, two of which are added with different amounts of stock solutions to prepare high and low concentration spiked samples, and establish a working curve. The measurement results are shown in Table (1):

[00...

Embodiment 2

[0024] Embodiment 2: the mensuration of triethylamine in weak alkaline water, solvent is dichloromethane.

[0025] First, dichloromethane was added to weakly alkaline water to adjust the pH value to strong alkalinity for extraction, and the lower dichloromethane layer was taken as the solution to be tested. Measure the density of triethylamine, dichloromethane and the solution to be tested, prepare 10ml of dichloromethane-triethylamine stock solution, the theoretical content of triethylamine in the stock solution is 5‰. Three parts of the solution to be tested were taken, two of which were added with different amounts of stock solution, prepared as high and low concentration spiked samples, and a working curve was established. The measurement results are shown in Table (2):

[0026] Table II)

[0027] serial number Determination of solution concentration ‰ Theoretical spiked concentration‰ Actual spiked concentration‰ Spike recovery % 1 0.32 0.73 0.6...

Embodiment 3

[0029] Embodiment 3: the mensuration of triethylamine in methylene chloride

[0030] Determination of the density of triethylamine, dichloromethane, triethylamine-dichloromethane solution, triethylamine-dichloromethane solution as the solution to be tested. Prepare 10ml of dichloromethane-triethylamine stock solution, the theoretical content of triethylamine in the stock solution is 20‰. Take three parts of the solution to be tested, two of which are added with different amounts of stock solution to prepare high and low concentration spiked samples, and establish a working curve. The measurement results are shown in Table (3):

[0031] Table (3)

[0032] serial number Determination of solution concentration ‰ Theoretical spiked concentration‰ Actual spiked concentration‰ Spike recovery % 1 38.01 9.51 10.41 109.46 2 38.31 9.51 10.71 112.62 3 26.69 10.02 10.52 104.99

[0033] Conclusion: As can be seen from the above table, the dev...

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Abstract

The invention relates to a method for determining the content of triethylamine in a solvent containing trace water by ultraviolet spectroscopy. The method comprises the following steps: (1) determining the density of triethylamine and the solvent; (2) preparing a solvent-triethylamine solution with unknown concentration as a control sample, and then preparing a stock solution of triethylamine and a solvent; and (3) taking three control samples with the same volume, respectively adding the stock solutions with different volumes to prepare standard samples with high, medium and low concentrations, scanning an ultraviolet spectrum in a wavelength range of 200-600nm by taking distilled water as a reference, and measuring the absorbance of each standard sample. And (4) calculating the concentration of triethylamine in the to-be-detected liquid according to the working curve, and determining the accuracy of the content of triethylamine in the to-be-detected liquid according to the standard recovery rate of the added standard sample. The method is simple to operate, high in timeliness, capable of rapidly and effectively determining low-content triethylamine, accurate and reliable in detection result and capable of meeting the requirements of actual production.

Description

technical field [0001] The invention belongs to the technical field of chemical detection and analysis, and in particular relates to a method for measuring the content of triethylamine in a solvent containing a small amount of water by ultraviolet spectroscopy. Background technique [0002] Triethylamine is a volatile organic amine, which may cause combustion and explosion hazards when exposed to open flames, high temperatures or strong oxidants. Slightly soluble in water, soluble in ethanol, ether and other organic solvents, it is a moderately toxic compound. In industry, it is mainly used as curing agent, catalyst, polymerization inhibitor and synthetic dye. It will have adverse effects on human production and life and industrial production. [0003] It is of great significance to study and establish a fast, accurate and simple analysis method for the content of triethylamine in organic solvent system (containing water). Gas chromatography is often used for the detectio...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N21/33G01N21/01
CPCG01N21/33G01N21/01
Inventor 张震孔波何爱晓卢主枫马瑞进崔杨周学祥李晓艳向玉杨英朝王建峰王新志
Owner 甘肃银光聚银化工有限公司