CN1417580A - Prepn of polyaniline coating for new-type solid microextracting head - Google Patents
Prepn of polyaniline coating for new-type solid microextracting head Download PDFInfo
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- CN1417580A CN1417580A CN 02153543 CN02153543A CN1417580A CN 1417580 A CN1417580 A CN 1417580A CN 02153543 CN02153543 CN 02153543 CN 02153543 A CN02153543 A CN 02153543A CN 1417580 A CN1417580 A CN 1417580A
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Abstract
The present invention belongs to the field of chemical analysis and measurement instrument, and relates to the development of solid microextracting coating. By means of chemical polymerization process, aniline monomer is made to polymer to the surface of stainless steel wire to form polyaniline coating. During preparation. Voltage and electroplating time are controlled to raise the the repeatability of coating preparation. The prepared coating has excellent selectivity to polar compound and no extraction effect on non-polar compound basically. Compared with available coating, the coating of the present invention has better mechanical and chemical stability, and no obvious change in extraction effect after being used in extraction inside strong alkali solution.
Description
The invention belongs to the field of chemical analysis and test instruments, and relates to a preparation method of a Solid Phase Microextraction (SPME) novel coating. And polymerizing the aniline monomer on the surface of the stainless steel wire by adopting an electrochemical polymerization method to form the polyaniline coating. During preparation, the repeatability of coating preparation is greatly improved by optimizing and controlling voltage and electroplating time. The prepared coating has good selectivity on polar compounds, and basically has no extraction effect on non-polar compounds. Compared with the existing commercial coating, the coating has better mechanical and chemical stability, and the extraction effect is not obviously changed after the coating is extracted in a strong alkaline solution (RSD is less than 5). The extraction head is suitable for extracting amines and alcohols in a complex matrix. Has good application prospect in the fields of environmental monitoring, food sanitation, inspection and quarantine, etc.
The background and current state of the art is generally as follows: the current commercial SPME coatings are mainly developed and produced by Supelco corporation. The SPME extraction head currently produced by the company coats a stationary phase coating on quartz fiber, wherein the coating comprises Polydimethylsiloxane (PDMS), polyethylene glycol/polydimethylsiloxane (CAR/PDMS), Polyacrylate (PA), carbon molecular sieve/vinyl benzene (CW/DVB) and carbon molecular sieve/molecular template resin (CW/TPR). These coatings are prepared by fixing high polymers on the surface of the quartz fiber by photocuring or high-temperature heating, and have poor mechanical and thermal stability, and in the case of direct extraction, the coatings are easily broken and peeled off, and the quartz fiber itself is easily broken. This limits its range of use and lifetime. In addition, to date, not a few researchers have developed more than twenty coatings. The best chemical stability is achieved by using sol-gel method, but this method has the problem of poor repeatability during coating, the 1999 Pawliszyn research group uses electrochemical polymerization method, using metal wire as working electrode, and puts its end into perchlorate acetonitrile solution containing pyrrole monomer, finally gets polypyrrole coating with positive charge on surface or inner wall, which can extract inorganic anion from water, and they also produce poly-N-phenylpyrrole coating by the same method. However, when the two coatings are applied to organic matter extraction, only nonpolar compounds can be extracted.
The invention adopts the novel polyaniline coating prepared by the electrochemical polymerization method to well overcome the defects, and uses the stainless steel wire to replace the quartz fiber to thoroughly overcome the defect that the quartz fiber is easy to be broken. The coating can extract inorganic anions from water, can also extract polar organic matters, and has good mechanical and chemical stability.
References to this can be found in: [1]belardi R P, Pawliszyn j.water polarization J canada.1990.24: 179-191[2]supra. chromatography products, sample handling: SPME.2000[3]J.C.Wu, X.M.Yu, H.Lord, J.Pawliszyn.Analyst.2000.125: 391-: 5001-5005[5]S.L.Chong, D.wang, J.D.Hayes, B.W.Wilhite, A.Malik.anal.chem, 1997.69: 3889 and 3898[6]T.P.Gbautu, K.L.Sutton, J.A.Caruso.anal Chim Acta, 1999.402: 67-79
The invention mainly aims to prepare the SPME novel coating by adopting a novel process, has better selectivity on polar organic matters, and completely meets the requirements of quantitative analysis on stability and repeatability. The technical scheme of the invention is realized by the following steps. FIG. 1 shows the structure of a solid phase micro-extraction head (wherein 1 is a plastic screw, 2 is a spring, 3 is a sealing gasket, 4 is an outer tube, 5 is an inner tube, 6 is a polyaniline coating, and 7 stainless steel wires). In electrochemical polymerization, we used a three-electrode system, where stainless steel wire was the working electrode, platinum electrode was the counter electrode, and calomel electrode was the reference electrode. The electrolyte is 1mol/L sulfuric acid solution containing 0.05mol/L aniline monomer. The stainless steel wire used was first polished with parchment paper and then ultrasonically cleaned in an ethanol solution for five minutes. The voltage is constant at 0.8V in the electroplating process, and the electroplating time is 3 hours. After the electroplating, a uniform black polyaniline coating is formed on the surface of the stainless steel wire. And (3) placing the newly prepared coating in a methanol solution for ultrasonic cleaning for three minutes, then placing the coating in a gas chromatography sample inlet, blowing the coating for 1 hour by using nitrogen, heating to 250 ℃, and aging for 1 hour.
Compared with the existing coating, the invention mainly has the following advantages:
1. because the electroplating device with optimized parameters is adopted to control the electroplating process, the process for preparing the coating is not only simple, but also has excellent repeatability.
2. The prepared coating is uniform and has good chemical and mechanical stability. The coating is cleaned by ultrasonic wave with organic solvent immediately after being prepared, and the coating does not break or peel.
3. In the course of the present invention we have not only repeatedly tested its stability, but also examined its selectivity. The first set of samples examined was 1mg/L BTEX (benzene, toluene, ethylbenzene and xylene) solution. After the polyaniline extraction head performs hollow extraction on the sample item for a certain time, the height of the polyaniline extraction head is higher in a gas chromatography vaporization chamberAnd (4) performing temperature analysis. The chromatographic column is HP-1, and the column temperature is as follows:
the FID detector temperature was 280 ℃. As a result, the polyaniline extraction head was found to have no extraction effect on BTEX. The second group of samples are mixed solution of 1mg/L ethanol, normal hexane and aniline, the mixed solution is extracted by a polyaniline extraction head in a headspace manner, the mixed solution is analyzed at high temperature in a gas chromatography vaporization chamber, a chromatographic column is still HP-1, and the temperature programming is adopted: the FID detector temperature was 280 ℃ and the spectrum is shown in FIG. 2(A is aniline).
And compared with CAR/DVB extraction head of Supelco company, the experimental conditions except temperature programming are changed into: the other conditions were not changed, and the spectrum is shown in FIG. 3(A is aniline).
It can be seen that the polyaniline extraction head has extraction effect only on polar substances (such as alcohols and amines). And the enrichment effect of the polyaniline extraction head on aniline is twice as high as that of CAR/DVB extraction head of Sullco company. The influencing parameters of the experiment and the RSD (<5%) were investigated for aniline. The optimized extraction conditions of aniline are that the sample volume is 10ml, when the extraction flask is 50ml, the pH value of the solution is more than 13, and the added NaCl is 4.00 g.
Claims (3)
1. The method is characterized in that the selectivity of the polyaniline is higher than that of a common commercial coating, the polyaniline has better selectivity to polar organic compounds in a complex system, and the extraction head is not easy to break.
2. The process of claim 1, wherein the stainless steel wire isused in place of the quartz fiber wire, and the stainless steel wire is not easily broken during the extraction process.
3. According to the method disclosed by claim 1, electrochemical polymerization is adopted in the preparation process, the process is simple, and the repeatability of the coating preparation is good.
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| Application Number | Priority Date | Filing Date | Title |
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| CN 02153543 CN1417580A (en) | 2002-12-04 | 2002-12-04 | Prepn of polyaniline coating for new-type solid microextracting head |
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| CN 02153543 CN1417580A (en) | 2002-12-04 | 2002-12-04 | Prepn of polyaniline coating for new-type solid microextracting head |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100418622C (en) * | 2006-03-28 | 2008-09-17 | 南京大学 | A novel solid-phase micro-extraction head with polythiophene and preparation method thereof |
| CN101468306A (en) * | 2007-12-29 | 2009-07-01 | 中国科学院生态环境研究中心 | Titanium-containing solid phase micro-extraction head and preparation method thereof |
| CN101294937B (en) * | 2008-06-12 | 2011-08-31 | 上海交通大学 | Electro-adsorption reinforced activated carbon fiber solid phase micro-extraction method |
| CN104138749A (en) * | 2014-07-21 | 2014-11-12 | 浙江大学 | Doped polyaniline solid phase microextraction fiber preparation method and application |
| CN108469489A (en) * | 2018-02-12 | 2018-08-31 | 东南大学 | A kind of highly polar matter selective separation enrichment pretreatment reagent kit and its application |
| CN110118839A (en) * | 2019-06-03 | 2019-08-13 | 红河学院 | The GC/MS fingerprint map construction method and its application of oldenlandia diffusa |
| CN110681184A (en) * | 2019-09-29 | 2020-01-14 | 华中师范大学 | Multi-walled carbon nanotube/polyaniline composite coating based in-pipe solid phase micro-extraction column and online micro-extraction method |
-
2002
- 2002-12-04 CN CN 02153543 patent/CN1417580A/en active Pending
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100418622C (en) * | 2006-03-28 | 2008-09-17 | 南京大学 | A novel solid-phase micro-extraction head with polythiophene and preparation method thereof |
| CN101468306A (en) * | 2007-12-29 | 2009-07-01 | 中国科学院生态环境研究中心 | Titanium-containing solid phase micro-extraction head and preparation method thereof |
| CN101294937B (en) * | 2008-06-12 | 2011-08-31 | 上海交通大学 | Electro-adsorption reinforced activated carbon fiber solid phase micro-extraction method |
| CN104138749A (en) * | 2014-07-21 | 2014-11-12 | 浙江大学 | Doped polyaniline solid phase microextraction fiber preparation method and application |
| CN104138749B (en) * | 2014-07-21 | 2017-12-15 | 浙江大学 | A kind of preparation method and application of doped polyaniline solid-phase micro-extraction fibre |
| CN108469489A (en) * | 2018-02-12 | 2018-08-31 | 东南大学 | A kind of highly polar matter selective separation enrichment pretreatment reagent kit and its application |
| CN110118839A (en) * | 2019-06-03 | 2019-08-13 | 红河学院 | The GC/MS fingerprint map construction method and its application of oldenlandia diffusa |
| CN110118839B (en) * | 2019-06-03 | 2022-02-18 | 红河学院 | Construction method and application of GC/MS (gas chromatography/mass spectrometry) fingerprint spectrum of oldenlandia diffusa |
| CN110681184A (en) * | 2019-09-29 | 2020-01-14 | 华中师范大学 | Multi-walled carbon nanotube/polyaniline composite coating based in-pipe solid phase micro-extraction column and online micro-extraction method |
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