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Method for preparing perfluorinated silane modified magnetic extraction stirring stick

A technology of perfluorosilane and magnetic stirring, which is applied in the field of trace analysis of organic pollutants, can solve problems such as temperature limitation and coating fracture, and achieve the effect of simple operation, low cost and strong adsorption force

Inactive Publication Date: 2013-06-26
SHAANXI NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Recently, a sol-gel method has been used to prepare perfluorinated capillary monolithic columns. The column prepared by this method has a certain adsorption capacity and selectivity for perfluorinated acid compounds, but due to a large number of perfluorinated groups embedded in the coating Inner, and the disadvantage of the sol-gel method is that the coating is prone to breakage, and there are restrictions on temperature and other conditions during use.

Method used

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  • Method for preparing perfluorinated silane modified magnetic extraction stirring stick
  • Method for preparing perfluorinated silane modified magnetic extraction stirring stick
  • Method for preparing perfluorinated silane modified magnetic extraction stirring stick

Examples

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Effect test

Embodiment 1

[0022] The steps of the preparation method of the perfluorosilane-modified magnetic extraction stirring bar of this embodiment are as follows:

[0023] 1. Prepare a magnetic stirring bar

[0024] Select a glass tube 1 with a length of 2 cm and an inner diameter of 2 mm, seal and package an iron core 2 with an outer diameter of 2 mm in the glass tube 1 and seal both ends of the glass tube 1 with an alcohol blowtorch to prepare a magnetic stirring bar. The specific length of the glass tube 1 can be arbitrarily selected in the range of 2 to 3 cm, and the inner diameter can be in the range of 2 to 4 mm. The outer diameter of the iron core 2 can also be slightly smaller than the inner diameter of the glass tube 1. When the glass tube 1 cannot move, the iron core 2 The length is less than the length of the glass tube 1.

[0025] 2. Surface pretreatment of magnetic stirring bar

[0026] The outer surface of the magnetic stirring rod is treated with dichloromethane for 20-30 minutes...

Embodiment 2

[0030] The steps of the preparation method of the perfluorosilane-modified magnetic extraction stirring bar of this embodiment are as follows:

[0031] In the surface pretreatment step 2 of the magnetic stirring bar, the outer surface of the magnetic stirring bar is treated with dichloromethane for 20-30 minutes, soaked in 1mol / L NaOH aqueous solution for 6-12 hours, and soaked in 0.1mol / L HCl aqueous solution for 1-2 hours. After 3 hours, wash with deionized water until neutral, place in a vacuum drying oven at 80°C, and dry at a vacuum of 0.06MPa for 3 hours.

[0032] In step 3 of preparing a perfluorosilane-modified magnetic extraction stir bar, place the pretreated magnetic stir bar in 5 mL of 1.71 mg / mL 1H,1H,2H,2H-perfluorodecyltrichlorosilane toluene solution , react for 5 hours at 50°C and a vacuum of 0.05MPa, a perfluorosilane layer 3 is formed on the surface of the glass tube 1, take out the magnetic stirring bar, place it in a vacuum drying oven, and dry at 50°C and...

Embodiment 3

[0035] The steps of the preparation method of the perfluorosilane-modified magnetic extraction stirring bar of this embodiment are as follows:

[0036]In the surface pretreatment step 2 of the magnetic stirring bar, the outer surface of the magnetic stirring bar is treated with dichloromethane for 20-30 minutes, soaked in 1mol / L NaOH aqueous solution for 6-12 hours, and soaked in 0.1mol / L HCl aqueous solution for 1-2 hours. After 3 hours, wash with deionized water until neutral, place in a vacuum drying oven at 100°C, and dry at a vacuum of 0.05MPa for 1 hour.

[0037] In step 3 of preparing a perfluorosilane-modified magnetic extraction stir bar, place the pretreated magnetic stir bar in 5 mL of 1.71 mg / mL 1H,1H,2H,2H-perfluorodecyltrichlorosilane toluene solution , react at 90°C and a vacuum of 0.05MPa for 5 hours, a perfluorosilane layer 3 is formed on the surface of the glass tube 1, take out the magnetic stirring bar, place it in a vacuum drying oven, and dry at 50°C and ...

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Abstract

The invention discloses a method for preparing a perfluorinated silane modified magnetic extraction stirring stick. The method comprises the following steps of: preparing a magnetic stirring stick, pretreating the surface of the magnetic stirring stick and preparing the perfluorinated silane modified magnetic extraction stirring stick. The perfluorinated silane modified magnetic extraction stirring stick is prepared by mutual action between fluorine and fluorine; competitive adsorption of stirrers during fiber solid-phase micro extraction is avoided; the volume of extraction solid phase is 50 times more than that of the solid-phase micro extraction; the enrichment time is obviously improved; the adsorption property is high; the selectivity is high; the low efficiency and non-selectivity of enrichment in a complicated substrate are avoided; perfluorinated compounds can be specifically and selectively extracted and separated; and trace analysis is facilitated.

Description

technical field [0001] The invention belongs to the technical field of trace analysis of organic pollutants, and in particular relates to a perfluorosilanized magnetic extraction stirring bar used for trace analysis of perfluorinated acid compounds in environmental samples. Background technique [0002] The currently reported separation and enrichment methods for perfluorinated compounds are mainly liquid-liquid extraction, liquid-solid extraction, or using commercial SPE columns (HLB solid-phase extraction column and WAX solid-phase extraction column from Waters Oasis, Varian The company's C18 solid-phase extraction column, etc. Although these enrichment methods can achieve better results to a certain extent, they do not have high selectivity. When dealing with large-volume environmental water samples with complex matrices, liquid-liquid extraction and the application of solid-phase extraction column technology are subject to certain restrictions. Curran et al. prepared a f...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/22B01J20/28B01J20/30
Inventor 张志琪郝双利张婧曹晓涵史婷
Owner SHAANXI NORMAL UNIV
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