Saraji Mohammad, Mehrafza Narges
Department of Chemistry, Isfahan University of Technology, Isfahan 84156-83111, Iran.
Department of Chemistry, Isfahan University of Technology, Isfahan 84156-83111, Iran.
J Chromatogr A. 2016 Aug 19;1460:33-9. doi: 10.1016/j.chroma.2016.07.036. Epub 2016 Jul 15.
In this paper, a mesoporous carbon-ZrO2 nanocomposite was fabricated on a stainless steel wire for the first time and used as the solid-phase microextraction coating. The fiber was synthesized with the direct carbonization of a Zr-based metal organic framework. With the utilization of the metal organic framework as the precursor, no additional carbon source was used for the synthesis of the mesoporous carbon-ZrO2 nanocomposite coating. The fiber was applied for the determination of BTEX compounds (benzene, toluene, ethylbenzene and m, p-xylenes) in different water samples prior to gas chromatography-flame ionization detection. Such important experimental factors as synthesis time and temperature, salt concentration, equilibrium and extraction time, extraction temperature, desorption time and desorption temperature were studied and optimized. Good linearity in the concentration range of 0.2-200μgL(-1) and detection limits in the range of 0.05-0.56μgL(-1) was achieved for BTEX compounds. The intra- and inter-day relative standard deviations were in the range of 3.5-4.8% and 4.9-6.7%, respectively. The prepared fiber showed high capability for the analysis of BTEX compounds in different water and wastewater samples with good relative recoveries in the range of 93-107%.
本文首次在不锈钢丝上制备了介孔碳-ZrO₂纳米复合材料，并将其用作固相微萃取涂层。该纤维通过基于Zr的金属有机框架直接碳化合成。利用金属有机框架作为前驱体，在合成介孔碳-ZrO₂纳米复合涂层时无需额外使用碳源。该纤维用于在气相色谱-火焰离子化检测之前测定不同水样中的BTEX化合物（苯、甲苯、乙苯和间、对二甲苯）。研究并优化了合成时间和温度、盐浓度、平衡和萃取时间、萃取温度、解吸时间和解吸温度等重要实验因素。对于BTEX化合物，在0.2-200μgL⁻¹浓度范围内实现了良好的线性，检测限在0.05-0.56μgL⁻¹范围内。日内和日间相对标准偏差分别在3.5-4.8%和4.9-6.7%范围内。所制备的纤维对不同水和废水样品中的BTEX化合物具有高分析能力，相对回收率良好，在93-107%范围内。
