Bagheri Habib, Banihashemi Solmaz, Jelvani Samaneh
Environmental and Bio-Analytical Laboratories, Department of Chemistry, Sharif University of Technology, P.O. Box 11365-9516, Tehran, Iran.
Environmental and Bio-Analytical Laboratories, Department of Chemistry, Sharif University of Technology, P.O. Box 11365-9516, Tehran, Iran.
J Chromatogr A. 2016 Aug 19;1460:1-8. doi: 10.1016/j.chroma.2016.06.078. Epub 2016 Jun 28.
A nanocomposite consisting of polythiophene-silver was prepared and implemented as a desired sorbent for headspace needle trap extraction. Colloidal silver nanoparticles (Ag NPs) with narrow size distribution and high stability were synthesized in water-in-oil microemulsion. This simple procedure was adapted to prepare highly monodispersed Ag NPs, starting from an initial synthesis in sodium bis(2-ethylhexyl) sulfosuccinate (AOT) reverse micelles. Polythiophene (PT) was synthesized by chemical oxidative polymerization in the presence of anhydrous ferric chloride while its polymeric structure was confirmed by Fourier transform infrared spectrometry (FTIR). Eventually, the prepared PT was dispersed in an AOT/n-decane solution containing Ag NPs for 1h in which the NPs were adsorbed on the polymer surface. The dynamic light scattering (DLS) analysis of NPs solution revealed that the monodisperse Ag NPs have been synthesized successfully with the size distribution below 10nm. Other instrumentations such as scanning electron microscopy (SEM), energy dispersive spectroscopy (EDS) and atomic absorption spectrometry (AAS) confirmed the fabrication of the PT-Ag nanocomposite. The applicability of the synthesized sorbent was examined by needle trap extraction of some polycyclic aromatic hydrocarbons (PAHs) in aqueous samples in conjunction with gas chromatography-mass spectrometry detection (GC-MS). Important parameters influencing the extraction process were optimized. The linearity for all analytes was in the concentration range of 0.01-10ngmL(-1). The limits of detections were in the range of 0.002-0.01ngmL(-1), using time-scheduled selected ion monitoring (SIM) mode while the RSD% values (n=3) were all below 12%. The developed method was successfully applied to real water samples obtained from different rivers and Persian Gulf, while the relative recovery percentages were in the range of 85-103%.
制备了一种由聚噻吩-银组成的纳米复合材料，并将其用作顶空针捕集萃取所需的吸附剂。在油包水微乳液中合成了尺寸分布窄且稳定性高的胶体银纳米颗粒（Ag NPs）。该简单方法适用于制备高度单分散的Ag NPs，起始于在双（2-乙基己基）磺基琥珀酸钠（AOT）反胶束中的初始合成。在无水氯化铁存在下通过化学氧化聚合合成聚噻吩（PT），同时通过傅里叶变换红外光谱（FTIR）确认其聚合物结构。最终，将制备的PT分散在含有Ag NPs的AOT/正癸烷溶液中1小时，其中NPs吸附在聚合物表面。NPs溶液的动态光散射（DLS）分析表明，已成功合成尺寸分布低于10nm的单分散Ag NPs。扫描电子显微镜（SEM）、能量色散光谱（EDS）和原子吸收光谱（AAS）等其他仪器证实了PT-Ag纳米复合材料的制备。通过结合气相色谱-质谱检测（GC-MS）对水性样品中的一些多环芳烃（PAHs）进行针捕集萃取，考察了合成吸附剂的适用性。优化了影响萃取过程的重要参数。所有分析物的线性范围为0.01-10ngmL(-1)。使用定时选择离子监测（SIM）模式时，检测限在0.002-0.01ngmL(-1)范围内，而相对标准偏差（RSD%）值（n=3）均低于12%。所开发的方法成功应用于从不同河流和波斯湾采集的实际水样，相对回收率在85-103%范围内。
