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Novel solid phase micro extraction head and its preparation method

A solid-phase micro-extraction head, a new type of technology, applied in solvent extraction, separation methods, chemical instruments and methods, etc., can solve problems such as application scope limitation, and achieve the effects of simple structure, large adsorption capacity, and broad application prospects.

Inactive Publication Date: 2006-04-26
NANJING UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the patent mentions that it only has an extraction effect on polar substances (such as alcohols and amines), so its application range has been greatly limited.

Method used

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  • Novel solid phase micro extraction head and its preparation method
  • Novel solid phase micro extraction head and its preparation method
  • Novel solid phase micro extraction head and its preparation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] A metal wire 11 with a diameter of 0.35 mm is inserted into the injection device 12 to form a simple solid-phase microextraction device. One end of the wire is used as a working electrode, combined with a platinum counter electrode and a saturated calomel reference electrode to form three electrode system. Put this three-electrode system into 0.2M aniline + 0.5M sulfuric acid solution, in the range of -0.2~1.0V, 25~35mV s -1 Under certain conditions, the cycle is 10-20 cycles to obtain a black polyaniline coating 13 adhered to the surface of the electrode. Finally, rinse and wash with double distilled water and methanol solution for 1 to 2 minutes to make a polyaniline-coated extraction head. Before the first use of this solid-phase microextraction head, it is aged in a gas chromatography vaporization chamber at 200-280°C for 2-3 hours, until no impurity peak appears.

Embodiment 2

[0028] A metal wire 11 with a diameter of 0.25 mm is inserted into the injection device 12 to form a simple solid-phase microextraction device. One end of the wire is used as a working electrode, combined with a platinum counter electrode and a saturated calomel reference electrode to form three electrode system. Put this three-electrode system into a 0.2M aniline+0.5M hydrochloric acid solution, and oxidize it for 10 minutes at 0.6V to obtain a black polyaniline coating 13 adhered to the electrode surface. Finally, rinse and wash with double distilled water and methanol solution for 1 to 2 minutes to make a polyaniline-coated extraction head. Before the first use of this solid-phase microextraction head, it is aged in a gas chromatography vaporization chamber at 200-280°C for 2-3 hours, until no impurity peak appears.

Embodiment 3

[0030] Insert a metal wire with a diameter of 0.45 mm into the injection device to form a simple solid-phase microextraction device. One end of the wire is used as a working electrode, combined with a platinum counter electrode and a saturated calomel reference electrode to form a three-electrode system . Put this three-electrode system into 0.3M aniline + 0.5M sulfuric acid solution, and the current density of the sample is 0.2-10.0mA / cm in the constant current method 2 Polymerized at a high current density to obtain a black polyaniline coating adhered to the electrode surface. Finally, rinse and wash with double distilled water and methanol solution for 1 to 2 minutes to make a polyaniline-coated extraction head. Before the first use of this solid-phase microextraction head, it is aged in a gas chromatography vaporization chamber at 200-280°C for 2-3 hours, until no impurity peak appears.

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Abstract

A new solid micro-extraction bulk and its preparing method, belonging to the technique field of environmental monitoring device. Inserting the metal wire into the injection device to make it become simple solid micro-extraction bulk; employing the front end of the metal wire as working electrode, combining with the platinum sheet electrode and saturated calomel reference electrode to form a three electrode system; putting it to the acid solution containing amino-benzene; forming the polyaniline coating stick to the surface of the front end of the metal wire by using electrochemical method; washing with second distilled water and methanol solution, and getting the new micro-extraction bulk. The product possesses good extracting selectivity for the trace organic pollutant of polar, non-polar, volatile and involatile. The product possesses good physical and chemical stability and long durability comparing with the commercial coating. The extraction bulk is suit for the analysis of various organic substance in the complex example, and good application potential in the field of environmental monitoring, food safety, checking and quarantine inspection, and etc.

Description

1. Technical field [0001] The invention relates to a solid-phase micro-extraction head applied to the analysis of various environmental pollutants and a preparation method thereof. 2. Background technology [0002] Solid phase microextraction (SPME) is a sample pretreatment technique developed in the early 1990s. It has been deeply researched and widely used in the analysis of organic compounds, especially volatile and semi-volatile organic compounds, combined with a variety of analytical methods. However, the types of commercial SPME solid-phase coatings currently used for actual analysis are limited, and most of them rely on physical adsorption to coat the stationary phase on the surface of brittle quartz fibers, so the thermal stability is poor (use temperature 200-280 ° C) , the service life is short (generally about 40 to 100 times), and the price is expensive, which directly limits the application range of the SPME method. Therefore, the development of solid phase co...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01D11/00C25D13/08G01N30/56
Inventor 孙成李想钟明
Owner NANJING UNIV