Bagheri Habib, Babanezhad Esmaeil, Es-haghi Ali
Department of Chemistry, Sharif University of Technology, Tehran, Iran.
J Chromatogr A. 2007 Jun 8;1152(1-2):168-74. doi: 10.1016/j.chroma.2007.02.007. Epub 2007 Feb 8.
A fiber coating from polyaniline (PANI) was electrochemically prepared and employed for solid phase microextraction (SPME) of some polycyclic aromatic hydrocarbons (PAHs) from water samples. The PANI film was directly electrodeposited on the platinum wire surface in sulfuric acid solution using cyclic voltammetry (CV) technique. The applicability of this coating was assessed employing a laboratory-made SPME device and gas chromatography with mass spectrometry (GC-MS) for the extraction of some PAHs from the headspace of aqueous samples. Application of wider potential range in CV led to a PANI with more stability against the temperature. The homogeneity and the porous surface structure of the film were examined by the scanning electron microscopy (SEM). The study revealed that this polymer is a suitable SPME fiber coating for extracting the selected PAHs. Important parameters influencing the extraction process were optimized and an extraction time of 40 min at 40 degrees C gave maximum peak area, when the aqueous sample was added with NaCl (20%, w/v). The synthesis of the PANI can be carried out conveniently and in a reproducible manner while it is rather inexpensive and stable against most of organic solvents. The film thickness of PANI can be precisely controlled by the number of CV cycles. The resulting thickness was roughly 20 microm after 20 cycles. At the optimum conditions, the relative standard deviation (RSD) for a double distilled water spiked with selected PAHs at ppb level were 8.80-16.8% (n = 3) and detection limits for the studied compounds were between 0.1-6 pg mL(-1). The performance of PANI was, also, compared with a commercial solid coated-based SPME fiber, carbowax/divinylbenzene (CW/DVB), under similar experimental conditions.
通过电化学方法制备了聚苯胺(PANI)纤维涂层,并将其用于从水样中固相微萃取(SPME)某些多环芳烃(PAHs)。使用循环伏安法(CV)技术,将聚苯胺膜直接电沉积在硫酸溶液中的铂丝表面。采用自制的SPME装置和气相色谱-质谱联用(GC-MS)技术评估了该涂层从水样顶空中萃取某些多环芳烃的适用性。在CV中应用更宽的电位范围可得到对温度更稳定的聚苯胺。通过扫描电子显微镜(SEM)检查了膜的均匀性和多孔表面结构。研究表明,这种聚合物是萃取所选多环芳烃的合适SPME纤维涂层。优化了影响萃取过程的重要参数,当水样中加入NaCl(20%,w/v)时,在40℃下萃取40分钟可得到最大峰面积。聚苯胺的合成可以方便地以可重复的方式进行,而且成本相当低,并且对大多数有机溶剂稳定。聚苯胺的膜厚度可以通过CV循环次数精确控制。20次循环后,所得厚度约为20微米。在最佳条件下,加标至ppb水平的选定多环芳烃的双蒸水的相对标准偏差(RSD)为8.80 - 16.8%(n = 3),所研究化合物的检测限在0.1 - 6 pg mL⁻¹之间。在相似的实验条件下,还将聚苯胺的性能与商用的基于固体涂层的SPME纤维Carbowax/二乙烯基苯(CW/DVB)进行了比较。