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基于过氧化磺化聚吡咯的电化学控制固相微萃取(EC-SPME)。

Electrochemically controlled solid-phase microextraction (EC-SPME) based on overoxidized sulfonated polypyrrole.

作者信息

Tamer Uğur, Ertaş Nusret, Udum Yasemin A, Sahin Yücel, Pekmez Kadir, Yıldız Attila

机构信息

Gazi University, Faculty of Pharmacy, Central Research Laboratory, Etiler, 06330 Ankara, Turkey.

出版信息

Talanta. 2005 Jul 15;67(1):245-51. doi: 10.1016/j.talanta.2005.03.003. Epub 2005 Apr 14.

DOI:10.1016/j.talanta.2005.03.003
PMID:18970163
Abstract

A method for the extraction and selective determination of cations is proposed using electro-synthesized overoxidized sulfonated polypyrrole film. The polymer film is used for the selective extraction of trace levels of nickel and cadmium ions by solid-phase microextraction (SPME). The cation uptake and release properties of the overoxidized sulfonated polypyrrole film electrode were examined under both open circuit and controlled potential conditions for prospective applications in electrochemically controlled solid-phase microextraction. Increased extraction efficiency and selectivity toward cations were achieved in high saline content of water. Simple preparation of film coatings on a platinum wire was possible using a constant potential method. Applied positive and negative potentials facilitated the extraction and desorption of cations, respectively. Nickel and cadmium ions were desorbed into sample aliquot and determined by electrothermal atomic absorption spectrometry (ETAAS). The cation uptake and release mechanism is affected both by the cation exchange at the negative sulfonate and carboxylate moiety on the film and the altered solution pH occurring at the counter electrode caused by the applied potential. The method was validated using a standard reference material and tested for the determination of cadmium ion in commercial table salt samples.

摘要

提出了一种使用电合成的过氧化磺化聚吡咯膜提取和选择性测定阳离子的方法。该聚合物膜用于通过固相微萃取(SPME)选择性提取痕量的镍和镉离子。在开路和控制电位条件下,研究了过氧化磺化聚吡咯膜电极对阳离子的吸附和释放特性,以期应用于电化学控制的固相微萃取。在高盐含量的水中,提高了对阳离子的萃取效率和选择性。使用恒电位法可以在铂丝上简单地制备膜涂层。施加的正电位和负电位分别促进了阳离子的萃取和解吸。镍和镉离子解吸到样品等分试样中,并用石墨炉原子吸收光谱法(ETAAS)测定。阳离子的吸附和释放机制既受膜上负磺酸根和羧酸根基团处的阳离子交换影响,也受施加电位在对电极处引起的溶液pH变化影响。该方法使用标准参考物质进行了验证,并用于测定市售食盐样品中的镉离子。

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