Baktash Mohammad Yahya, Bagheri Habib
Environmental Bio-Analytical Laboratories, Department of Chemistry, Sharif University of Technology, P.O. Box 11365-9516, Tehran, Iran.
Environmental Bio-Analytical Laboratories, Department of Chemistry, Sharif University of Technology, P.O. Box 11365-9516, Tehran, Iran.
J Chromatogr A. 2017 Jun 2;1500:69-75. doi: 10.1016/j.chroma.2017.04.011. Epub 2017 Apr 8.
In this research, an attempt was made toward synthesizing a sol-gel-based silica aerogel and its subsequent coating on a copper wire by phase separation of polystyrene. Adaption of this new approach enabled us to coat the metallic wire with powder materials. The use of this method for coating, led to the formation of a porous and thick structure of silica aerogel. The coated wire was placed in a needle and used as the sorbent for in-tube solid phase microextraction of chlorobenzenes (CBs). The superhydrophobicity of sorbent on extraction efficiency was investigated by using different ratios of tetraethylorthosilicate/methyltrimethoxysilane. The surface coated with the prepared silica aerogel by the phase separation of polystyrene showed high contact angle, approving the desired superhydrophobic properties. Effects of major parameters influencing the extraction efficiency including the extraction temperature, extraction time, ionic strength, desorption time were investigated and optimized. The limits of detection and quantification of the method under the optimized condition were 0.1-1.2 and 0.4-4.1ngL, respectively. The relative standard deviations (RSD%) at a concentration level of 10ngL were between 4 and 10% (n=3). The calibration curves of CBs showed linearity from 1 to100ngL. Eventually, the method was successfully applied to the extraction of model compounds from real water samples and relative recoveries varied from 88 to 115%.
在本研究中,尝试通过聚苯乙烯的相分离合成基于溶胶 - 凝胶的二氧化硅气凝胶,并将其随后涂覆在铜线上。采用这种新方法使我们能够用粉末材料涂覆金属线。使用这种涂覆方法导致形成多孔且厚的二氧化硅气凝胶结构。将涂覆的金属线置于针中,并用作氯苯(CBs)管内固相微萃取的吸附剂。通过使用不同比例的正硅酸乙酯/甲基三甲氧基硅烷研究了吸附剂的超疏水性对萃取效率的影响。通过聚苯乙烯相分离制备的二氧化硅气凝胶涂覆的表面显示出高接触角,证实了所需的超疏水性能。研究并优化了影响萃取效率的主要参数,包括萃取温度、萃取时间、离子强度、解吸时间。在优化条件下该方法的检测限和定量限分别为0.1 - 1.2和0.4 - 4.1 ng/L。在10 ng/L浓度水平下的相对标准偏差(RSD%)在4%至10%之间(n = 3)。CBs的校准曲线在1至100 ng/L范围内呈线性。最终,该方法成功应用于从实际水样中萃取模型化合物,相对回收率在88%至115%之间。