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Preparation method of titanium oxide extraction bar for solid phase microextraction

A titanium oxide and extraction rod technology, which is applied in the field of preparation of new titanium oxide hollow fiber extraction rods, can solve the problems of weak resistance to solvent washing, low extraction and enrichment times, limited types of coatings, etc., and achieves chemical and thermal stability. Good, controllable coating thickness, wide application effect

Inactive Publication Date: 2010-06-30
LANZHOU INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, so far, the types of coatings for solid-phase microextraction tips are limited, the use temperature is low (200-280°C), the ability to resist solvent washing is weak, the service life is short, easy to break, and the extraction enrichment factor is low, which greatly limits its scope of application

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0013] Take 50ml of butyl titanate in a 100ml beaker, slowly add 15ml of acetic acid, then add 175ml of absolute ethanol, mix evenly with 200ml of absolute ethanol and 10ml of deionized water, slowly pour it into the beaker, stir it evenly with a magnetic force and place it in a sealed place Overnight, a 0.2 mol / L titanium sol was obtained.

[0014] The polypropylene hollow fiber was cut into small pieces of 7.5 mm, soaked in acetone and ultrasonically washed for 10 minutes, and then air-dried.

[0015] Immerse the above-mentioned polypropylene hollow fiber in 5ml of the prepared titanium sol, ultrasonically vibrate for 0.5 hours, let it stand for 2 hours, take it out and put it in a 393K oven to dry for 2 hours, repeat the impregnation process 10 times, and obtain a titanium oxide-coated polymer. Propylene hollow fiber extraction rods. Put it into a muffle furnace, control the temperature rise rate to 2K / min, and the calcination temperature to 798K, and maintain this tempera...

Embodiment 2

[0017] Take 10ml of butyl titanate in a 100ml beaker, slowly add 3ml of acetic acid, then add 44ml of absolute ethanol, draw 1ml of deionized water with a syringe, slowly pour it into the beaker, stir it evenly with a magnetic force, and seal it overnight to obtain 0.5mol / L of titanium sol.

[0018] The polypropylene hollow fiber was cut into 5mm small pieces, soaked in acetone and ultrasonically washed for 10 minutes, and then air-dried.

[0019] The above-mentioned polypropylene hollow fiber was immersed in 5ml of the prepared titanium sol, ultrasonically oscillated for 0.5 hours, left to stand for 2 hours, taken out and placed in a 393K oven to dry for 2 hours, and the impregnation process was repeated 6 times to obtain a titanium oxide-coated polymer. Propylene hollow fiber extraction rods. Put it into a muffle furnace, control the heating rate to 2K / min, and the calcination temperature to 823K, and maintain this temperature for 5 hours to obtain the finished titanium oxi...

Embodiment 3

[0021] The titanium oxide hollow fiber extraction rod prepared in Example 1 was used to extract and analyze N,N-dimethylacetamide in the water sample.

[0022] Put the titanium oxide hollow fiber extraction rod prepared in Example 1 into the water sample containing N,N-dimethylacetamide, extract by ultrasonic vibration for 3 hours, take out and dry the water, and use 50 microliters of absolute ethanol Desorb for 2 hours at room temperature, and the desorbed ethanol directly enters gas chromatography (GC-FID) for analysis.

[0023] Gas chromatography conditions: Agilent GC 6890, using AT SE-54 column (50×0.25×0.33); temperature program: initial temperature 160°C, heating rate 20°C / min, final temperature 250°C; carrier gas: nitrogen, pressure 17.16psi , splitless injection, hydrogen ion flame (FID) detector, the temperature of the front detector is 250 ℃.

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PUM

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Abstract

The invention discloses a preparation method of a titanium oxide extraction bar for solid phase microextraction; in the method, a plurality of titanium oxide layers are deposited on the surface of polypropylene hollow fiber by adopting a sol-gel method, and then polypropylene matrix is removed by high-temperature firing, so as to obtain the titanium oxide hollow fiber extraction bar, realize extraction preenrichment to polar compounds with micro and trace amount in medicine and environment samples and carry out separation analysis to gas chromatography or high performance liquid chromatography; the extraction bar has a three-dimensional porous stricture, has larger specific surface area, controllable coating thickness, good chemical and heat stability, wide pH stabilization range (pH=1-14) and high extraction efficiency to the polar compounds.

Description

technical field [0001] The invention relates to a preparation method of a novel titanium oxide hollow fiber extraction rod for solid-phase microextraction, in particular to a method for extraction and pre-enrichment of trace and trace polar compounds in samples such as food, medicine, environment, inspection and quarantine, etc. A method for preparing a titanium oxide hollow fiber extraction rod. Background technique [0002] Solid phase microextraction (SPME) (R.P, Belardi and Pawlisyn, Water Pollution Research J. Canada. 1989, 24, 179) has developed into a relatively mature sample pretreatment technique. This technology integrates sampling, extraction, concentration and sample injection. It has many advantages such as less sample consumption, almost no organic solvent, easy to combine with other analytical instruments, simple and fast operation, and compact device, so it is widely used in various sample detection. . However, so far, the types of coatings for solid-phase ...

Claims

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Application Information

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IPC IPC(8): B01J20/30
Inventor 师彦平李佳戚欢阳
Owner LANZHOU INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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