Behzadi Mansoureh, Mirzaei Mohammad
Department of Chemistry, Shahid Bahonar University of Kerman, P.O. Box 76169-133, Kerman, Iran.
Department of Chemistry, Shahid Bahonar University of Kerman, P.O. Box 76169-133, Kerman, Iran; Department of Environment, Graduate University of Advanced Technology, P.O. Box 763113-3131, Kerman, Iran.
J Chromatogr A. 2016 Apr 22;1443:35-42. doi: 10.1016/j.chroma.2016.03.039. Epub 2016 Mar 17.
A poly(o-anisidine)/graphene oxide nanosheets (PoA/GONSs) coating is fabricated by a simple and efficient electrochemical deposition method on steel wire. The incorporation of PoA and GONSs allows preparing a nanocomposite that can successfully integrate the advantages of both. Then, the prepared fiber is applied to the headspace solid-phase microextraction (HS-SPME) and gas chromatographic analysis of benzene, toluene, ethylbenzene and xylenes. In order to obtain an adherent, stable and efficient fiber to extract target analytes, experimental parameters related to the coating process such as deposition potential, deposition time, concentration of the monomer and concentration of GONSs were studied. The prepared composite fiber were characterized by Fourier transform infrared spectroscopy, powder X-ray diffraction and scanning electron microscopy. The effect of various parameters on the efficiency of HS-SPME process consisting of desorption temperature and time, extraction temperature and time and ionic strength were also optimized. Under the optimal conditions, the method was linear for orders of magnitude with correlation coefficients varying from 0.9888 to 0.9993. Intra- and inter-day precisions of the method were determined from mixed aqueous solutions containing 5.0 ng mL(-1) of each BTEX. The intra-day precisions varied from 3.1% for toluene to 5.7% for ethylbenzene, while the inter-day precisions varied from 4.9% for o-xylene to 7.3% for m,p-xylene. Limits of detection were in the range 0.01-0.06 ng mL(-1). The proposed method was applied to monitor BTEX compounds in some water samples and the accuracies found through spiking river water samples showed high recoveries between 92.0 and 101.2%.
通过一种简单高效的电化学沉积方法在钢丝上制备了聚(邻甲氧基苯胺)/氧化石墨烯纳米片(PoA/GONSs)涂层。PoA和GONSs的结合使得能够制备出一种纳米复合材料,该复合材料可以成功整合两者的优点。然后,将制备好的纤维应用于苯、甲苯、乙苯和二甲苯的顶空固相微萃取(HS-SPME)和气相色谱分析。为了获得一种能提取目标分析物的附着性好、稳定且高效的纤维,研究了与涂层过程相关的实验参数,如沉积电位、沉积时间、单体浓度和GONSs浓度。通过傅里叶变换红外光谱、粉末X射线衍射和扫描电子显微镜对制备的复合纤维进行了表征。还优化了各种参数对HS-SPME过程效率的影响,包括解吸温度和时间、萃取温度和时间以及离子强度。在最佳条件下,该方法在几个数量级上呈线性,相关系数在0.9888至0.9993之间。该方法的日内和日间精密度是由含有5.0 ng mL⁻¹每种BTEX的混合水溶液测定的。日内精密度从甲苯的3.1%到乙苯的5.7%不等,而日间精密度从邻二甲苯的4.9%到间二甲苯和对二甲苯的7.3%不等。检测限在0.01 - 0.06 ng mL⁻¹范围内。该方法应用于监测一些水样中的BTEX化合物,通过对河水样加标发现的准确度显示回收率在92.0%至101.2%之间,回收率较高。