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Integrated porous polymer adsorption extraction stirring bar and its manufacturing method

A technology of porous polymers and stirring rods, applied in the direction of selective adsorption, alkali metal compounds, chemical instruments and methods, etc., can solve the problems of limiting the sensitivity of sample analysis and the inability to use the depletion principle, etc., to achieve good mechanical properties and prolong service life , the effect of large extraction capacity

Inactive Publication Date: 2013-01-16
NINGBO UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the above research results are mainly extraction matrices prepared by free radical polymerization of olefin polymers, and it is difficult to obtain larger volumes of stirring rod adsorption extraction materials, which leads to the use of equilibrium principles based on solid-phase microextraction in the extraction process. The depletion principle used in solid phase extraction cannot be used, which limits the sensitivity of sample analysis

Method used

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  • Integrated porous polymer adsorption extraction stirring bar and its manufacturing method
  • Integrated porous polymer adsorption extraction stirring bar and its manufacturing method
  • Integrated porous polymer adsorption extraction stirring bar and its manufacturing method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] 1) Preparation of the stirring magnet: cut a section of 0.5mm stainless steel wire with a diameter of 10mm, clean it and dry it, then coat it with a commercially available acrylic modified epoxy or epoxy resin system glue, and wait until it is completely cured for later use.

[0024] 2) Preparation of stirring bar for adsorption extraction: Take 8.0g acrylonitrile, 0.6g ethylene glycol acrylate, 0.2g itaconic acid, 6.0g dimethylformamide, 10.0g caprolactam, 20mg azobisisobutyronitrile, mix uniform. Pour it into a 0.5mL stainless steel tube (the inner diameter of the tube is about 2.5mm), inject the liquid with a length of about 12mm, seal it and place it in a 60°C oven for 1 hour to react, dip the aforementioned stainless steel wire vertically into the center of the reaction system, seal it and put it in the React in an oven at 65°C for 12 hours, and take out the prepared stirring rod. The schematic diagram of the polymerization process and the molecular structure of t...

Embodiment 2

[0027] The preparation of the stirring magnet is the same as in Example 1.

[0028]Take 8.0g of acrylonitrile, 1.2g of ethylene glycol acrylate, 0.8g of itaconic acid, 4.0g of dimethylformamide, 12.0g of caprolactam, and 30mg of azobisisobutyronitrile, and mix them evenly. Pour it into a 1mL stainless steel tube (the inner diameter of the tube is about 5mm), inject the liquid with a length of about 16mm, seal it and place it in a 70°C oven for 0.5h, dip the aforementioned stainless steel wire vertically into the center of the reaction system, seal it and place it in the After reacting in an oven at 70°C for 6 hours, the prepared stirring rod was taken out, washed repeatedly with deionized water until the porogen was completely removed, and placed in deionized water for later use.

Embodiment 3

[0030] Prepare the copper ion standard solution, adjust the pH=5 and place it in a small beaker, put the stirring rod prepared according to Example 1, at room temperature at a speed of 200r min -1 Under adsorption extraction for 20min, take out the stirring rod. with 2 mL of 5% HNO 3 Analyze at a certain stirring speed, and measure the ion concentration in the eluent by atomic emission spectrometry, and select 324.754nm as the measuring wavelength. The recovery rate of the standard addition reached over 98%, the relative standard deviation was 4.1%, and the detection limit was 3.2ng mL -1 .

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Abstract

The invention relates to an integrated porous polymer adsorption extraction stirring bar and its manufacturing method. The stirring bar comprises a stirring magneton and a coat coated outside the stirring magneton, wherein the coat is an acrylonitrile-ethylene glycol acrylate-itaconic acid copolymer. A mixed solvent of dimethyl formamide and caprolactam is added to a reaction system as a pore forming agent, azodiisobutyronitrile is used to carry out thermal initiation of an in-situ free radical polymerization reaction, and a prepared integrated porous material is adopted as the coat of the adsorption extraction stirring bar, so the adsorption extraction stirring bar has the advantages of rapid adsorption and desorption rates, large extraction capacity, and realization of the adoption of an equilibrium extraction mode of solid phase micro-extraction or a depleted extraction mode of solid phase extraction. The ethylene glycol acrylate which is a crosslinking agent improves the mechanical performances of the coat of the stirring bar and prolong the service life. The itaconic acid which is a modifier makes the extraction coat contain a plurality of carboxyl groups, and can directly adsorb and extract parts of heavy metal cations and polar organic compounds. The preparation method is simple and can be easily operated.

Description

technical field [0001] The present invention relates to an adsorption extraction stirring rod, in particular to a stirring rod for solid phase extraction based on a porous material of integral acrylonitrile-ethylene glycol acrylate-itaconic acid terpolymer and a preparation method thereof, It belongs to the technical field of analytical chemistry sample pretreatment, and is suitable for the pretreatment of complex samples such as food and environment. Background technique [0002] The stir bar (stir bar) that is used for adsorption extraction was proposed by Baltussen E et al. based on solid phase microextraction (SPME) technology in 1999 (Baltussen E, Sandra P, David F, Cramers C, J.microcolumn sep. 1999, 11(10): 737-747), and commercialized by Gerstel GmbH (Frank D, Tienpont B, Sandra P. LC-GC North America, 2003.21(2): 1-7). Compared with the traditional fiber-needle solid-phase microextraction head, because it can complete the stirring itself and accelerate the mass tra...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/26B01J20/28B01J20/32B01D15/08G01N1/34G01N1/40
Inventor 王邃危晶郭智勇
Owner NINGBO UNIV
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