聚苯乙烯/氧化锆固相萃取填料的制备及江水中硫双二氯酚的测定  

Preparation of polystyrene-zirconia composite solid-phase extraction filler and determination of bithionol in the river

作　　者：江艳[1] 马柏凤[1] 

机构地区：[1]齐齐哈尔大学化学与化学工程学院,黑龙江齐齐哈尔161006

出　　处：《齐齐哈尔大学学报（自然科学版）》2014年第6期76-79,共4页Journal of Qiqihar University(Natural Science Edition)

基　　金：黑龙江省自然科学基金资助项目(B201101)

摘　　要：制备了二氧化锆微球,并用硅烷偶联剂处理得到乙烯基二氧化锆。通过自由基聚合,苯乙烯、二乙烯基苯与乙烯基二氧化锆颗粒反应,将交联聚苯乙烯包覆在锆基质表面上,制得聚苯乙烯/氧化锆基质固相萃取柱填料,并对其结构和形貌进行了表征。用该填料制备固相萃取小柱,对江水中的硫双二氯酚进行萃取,乙腈为洗脱剂,洗脱液用于液相色谱分析。分别考察了样品的p H值和流速、洗脱剂的体积和流速对萃取回收率的影响,确定了最佳固相萃取条件及最佳色谱分析条件。结果表明,聚苯乙烯/氧化锆复合微球具有均一的分散性,而且自制固相萃取小柱对江水中的硫双二氯酚吸附性能好,与HPLC联用测定结果重现性也好,最低检测限为0.31μg/L。In this paper, zirconia microspheres synthetized was treated by vinyl-silane coupling agent to get vinyl-zirconia.The SPE filler of cross-linked polystyrene encapsulated zirconia-base was synthesized by styrene,divinylbenzene and vinyl-zirconia through radical polymerization,and the structure and morphology of the filler was observed. The composite microspheres were used as solid-phase extraction（SPE）sorbents to selectively extract bithionol in the river.Acetonitrile was used as eluent, and the eluate was determined by high performance liquid chromatography. The effects of the sample flow rate and pH, volume and flow rate of eluent on adsorption ratios were investigated, the best conditions of solid phase extraction and HPLC were obtained. The result shows that composite microspheres synthetized have a uniform monodispersity in particle size. The SPE sorbents is of good adsorption performance to bithionol in the river, and the reproducibility of determining method of SPE-HPLC for the bithionol is good, the detection limits for bithionol was 0.31μg/L.

关 键 词：聚苯乙烯/氧化锆 固相萃取填料 高效液相色谱 硫双二氯酚 

分 类 号：O652.63[理学—分析化学]