Polyaniline solid phase micro- extraction head and method for making same

A technology of solid-phase microextraction head and polyaniline, which is applied in the direction of chemical instruments and methods, preparation of test samples, and other chemical processes, can solve the problems of short service life and high price of solid-phase microextraction head, and achieve mechanical The effect of superior strength, low price, and good physical stability

Inactive Publication Date: 2008-10-22
NANJING UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] 1. The technical problem to be solved by the invention: Aiming at the short service life and high price of the existing solid-phase microextraction head, the present invention provides a polyaniline solid-phase microextraction head and a preparation method thereof, and the prepared polyaniline solid-phase microextraction head The phase microextraction head is used for the fast, simple and sensitive green pretreatment of SPME of polychlorinated biphenyls, polycyclic aromatic hydrocarbons and phthalates

Method used

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  • Polyaniline solid phase micro- extraction head and method for making same
  • Polyaniline solid phase micro- extraction head and method for making same
  • Polyaniline solid phase micro- extraction head and method for making same

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Effect test

Embodiment 1

[0021] The stainless steel wire (diameter 0.35mm, length 75mm) was ground to 0.1mm at the front end 1cm, and this was used as the working electrode, the platinum sheet was used as the counter electrode, and the saturated calomel electrode was used as the reference electrode. Put it into a water-acetonitrile (V:V=49:1) solution containing 0.2M aniline and 0.5M trifluoroacetic acid, within the range of -0.2 to 1.2V, 25mVs -1 Cycle a certain number of times until the power is 1C, and keep it at 1.2V for 5s. Immerse in methanol for 100s, wash with deionized water for 10s, repeat twice. Vacuum-dried at 80°C for 5 hours, cross-linked at 125°C for 5 hours, and baked and aged at high temperature (280°C) for 2 hours in a gas chromatography inlet to make polyaniline solid-phase microextraction tips (fibers).

[0022] figure 1 : SEM of a polyaniline solid-phase microextraction head (left: 300X, right: 5000X). The scanning electron microscope atlas shows that the extraction head is uni...

Embodiment 2

[0028] The stainless steel wire (0.35 mm in diameter, 75 mm in length) was ground to a diameter of 0.12 mm at the front end 1 cm, and this was used as the working electrode, the platinum sheet was used as the counter electrode, and the saturated calomel electrode was used as the reference electrode. Put it into the trifluoroacetic acid solution containing 0.2M aniline, in the range of -0.2 ~ 1.2V, 25mV s -1 Cycle a certain number of times until the power is 1C, and keep it at 1.2V for 5s. Immerse in ethanol for 300s, wash in deionized water for 10s, repeat twice. Vacuum-dried at 80°C for 5 hours, cross-linked at 150°C for 2 hours, and then baked and aged at high temperature (200°C) for 2 hours in a gas chromatography inlet to make a polyaniline solid-phase microextraction tip (fiber).

[0029] figure 2 Comparison of the optimized extraction efficiency of polyaniline solid-phase microextraction head (fiber) for 6 kinds of polychlorinated biphenyls (concentration is 6.66ppt),...

Embodiment 3

[0038] The stainless steel wire (0.35mm in diameter, 75mm in length) was ground to a diameter of 0.11mm at the front end 1.5cm, and this was used as the working electrode, the platinum sheet was used as the counter electrode, and the saturated calomel electrode was used as the reference electrode. Put it in a water-acetonitrile (V:V=20:1) solution containing 0.2M aniline and 0.5M trifluoroacetic acid, within the range of -0.2 to 1.2V, 20mV s -1 Cycle a certain number of times until the power is 1C, and keep it at 1.2V for 5s. Immerse in dichloromethane for 60s, wash with deionized water for 10s, repeat twice. Vacuum-dried at 80°C for 5 hours, cross-linked at 130°C for 3 hours, and then baked and aged at high temperature (250°C) for 3 hours in a gas chromatography inlet to make a polyaniline solid-phase microextraction tip (fiber).

[0039] Extraction of 10 kinds of normal alkanes, phenanthrene, pyrene and dibutyl phthalate.

[0040] GC / FID operating conditions:

[0041] Pro...

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Abstract

The invention discloses a polyaniline solid-phase micro-extraction head and a method for preparing the same. The method is as follows: an aniline monomer is made to generate electrochemical polymerization reaction on the surface of a metal head by utilization of the electrochemical method and then a polymer coating with extraction ability is formed on the surface of the metal head through regulating and controlling coating preparation conditions; the method uses 0.5 to 1.5 centimeter of the front end of a wire as a working electrode, a platinum sheet as a counter electrode and a saturated calomel electrode as a reference electrode; the electrodes are placed into 0.2M aniline-trifluoroacetic acid solution of electrolyte; the cyclic voltammetry is adopted and the scanning speed is not more than 0.025 mV/s; a prepared extraction head is steeped in organic solvent such as methanol, ethanol, toluene, methylene dichloride and so on; the extraction head is roasted for 2 to 5 hours at a temperature of between 125 and 150 DEG C and roasted for 2 to 5 hours at a temperature between 200 and 280 DEG C, and then the high-efficient solid-phase extraction head is prepared. The polyaniline solid-phase micro-extraction head prepared has high extraction efficiency, meets the requirements of trace amount analysis, and is used for quick, simple, convenient and high-sensitive green preliminary treatment of SPMEs of polychlorobiphenyl, polycyclic aromatic hydrocarbon and phthalate esters.

Description

technical field [0001] The invention relates to a solid-phase micro-extraction head used for pretreatment in the monitoring method of organic pollutants of polychlorinated biphenyls, polycyclic aromatic hydrocarbons and phthalates in water bodies and a preparation method thereof. Background technique [0002] Sample pretreatment plays a pivotal role in the sample analysis process, which is directly related to the sensitivity, reliability and analysis speed of the analysis results. Environmental samples are low in concentration and require an appropriate enrichment step. At present, solid phase extraction is mostly used. This technology has a simple device, a small amount of solvent, and can perform automatic control and on-site analysis. However, the operation is cumbersome, the influence of the matrix is ​​large, the blank value is high, and the adsorption column is easily blocked, which leads to unsatisfactory reproducibility. For example, The contamination of phthalate e...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/08G01N1/40B01J20/30
Inventor 孙成王永花张娟郭会琴陈广春张莉杨绍贵
Owner NANJING UNIV
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