Behfar Mina, Ghiasvand Ali Reza, Yazdankhah Fatemeh
Department of Chemistry, Lorestan University, Khoramabad, Iran.
J Sep Sci. 2017 Jul;40(14):2975-2983. doi: 10.1002/jssc.201700244. Epub 2017 Jun 19.
The surface of a stainless-steel wire was platinized using electrophoretic deposition method to create a high-surface-area with porous and cohesive substrate. The platinized fiber was coated by the polypyrrole/graphene oxide nanocomposite by electropolymerization and accommodated into a stainless-steel needle to fabricate an in-needle coated fiber. The developed setup was coupled to gas chromatography with flame ionization detection and applied to extract and determine polycyclic aromatic hydrocarbons (naphthalene, fluorene, phenanthrene, fluoranthene, and pyrene) in complicated solid matrices, along with reinforcement of the extraction by cooling the sorbent, using liquid carbon dioxide. To obtain the best extraction efficiency, the important experimental variables including extraction temperature and time, temperature of cooled sorbent, sampling flow rate, and desorption condition were studied. Under the optimal condition, limits of detection for five studied analytes were in the range of 0.2-0.8 pg/g. Linear dynamic ranges for the calibration curves were found to be in the range of 0.001-1000 ng/g. Relative standard deviations obtained for six replicated analyses of 1 ng/g of analytes were 4.9-13.5%. The reinforced in-needle coated fiber method was successfully applied for the analysis of polycyclic aromatic hydrocarbons in contaminated soil samples.
采用电泳沉积法对不锈钢丝表面进行镀铂处理，以制备具有高表面积的多孔且有粘性的基底。通过电聚合将聚吡咯/氧化石墨烯纳米复合材料涂覆在镀铂纤维上，并将其装入不锈钢针中，制成针内涂覆纤维。所开发的装置与带有火焰离子化检测的气相色谱联用，用于在复杂固体基质中萃取和测定多环芳烃（萘、芴、菲、荧蒽和芘），同时通过使用液态二氧化碳冷却吸附剂来加强萃取效果。为了获得最佳萃取效率，研究了包括萃取温度和时间、冷却吸附剂的温度、采样流速和解吸条件等重要实验变量。在最佳条件下，五种研究分析物的检测限在0.2 - 0.8 pg/g范围内。校准曲线的线性动态范围为0.001 - 1000 ng/g。对1 ng/g分析物进行六次重复分析得到的相对标准偏差为4.9 - 13.5%。强化针内涂覆纤维法成功应用于污染土壤样品中多环芳烃的分析。
