双硫腙/凹凸棒土复合固相萃取填料的制备及其对重金属离子吸附性能的研究  

Study on preparation of composite dithizone/attapulgite solid phase extraction packingandits adsorption properties for heavy metal ions

作　　者：杨雪 申书昌[1] YANG Xue;SHEN Shuchang(Center of Analysis and Testing,Qiqihar University,Qiqihar 161006,China)

机构地区：[1]齐齐哈尔大学分析测试中心,黑龙江齐齐哈尔161006

出　　处：《高师理科学刊》2021年第4期49-56,共8页Journal of Science of Teachers＇College and University

摘　　要：通过对凹凸棒土进行盐酸预处理、苯基三甲氧基硅烷表面改性和复合双硫腙,制备了复合固相萃取填料(DZ@ATP).采用扫描电子显微镜(SEM)、X射线能谱仪(EDS)、傅里叶变换红外光谱仪(FI-IR)、X射线光电子能谱仪(XPS)对其进行表征,确定了最佳固相萃取条件.考察了DZ@ATP对水中Cd2^(+),Co2^(+),Cu2^(^(+)),Cr3^(+),Pb2^(+),Sb3^(+),Sn2^(+),Tl^(+),Zn2^(+),Tb3^(+),Ag^(+),Hg2^(+)的吸附性能.吸附容量分别达到15.99,13.45,14.72,12.97,15.77,13.15,14.93,13.81,14.09,13.11,15.82,14.98 mg/g.通过固相萃取与电感耦合等离子体质谱仪(ICP-MS)联用测定了水样中重金属离子的含量,检出限分别为0.041,0.027,0.033,0.047,0.063,0.017,0.052,0.084,0.019,0.018,0.056,0.040μg/L.The compound solid phase extraction packing(DZ@ATP)was prepared by the pretreatment of hydrochloric acid,the surface modification of phenyltrimethoxysilaneand compound of dithizone to attapulgite.Then DZ@ATP was characterized by SEM,EDS,FT-IR and XPS.And the optimum solid phase extraction conditions were determined.The adsorption performance of DZ@ATP packing on Cd2^(+),Co2^(+),Cu2^(+),Cr3^(+),Pb2^(+),Sb3^(+),Sn2^(+),Tl^(+),Zn2^(+),Tb3^(+),Ag^(+),Hg2^(+)was investigated.The saturated adsorption capacity of the DZ@BATP for heavy metal ions were 15.99,13.45,14.72,12.97,15.77,13.15,14.93,13.81,14.09,13.11,15.82,14.98 mg/g.The contents of heavy metal ions in the water sample were determined by solid phase extraction and ICP-MS.The detection limits were 0.041,0.027,0.033,0.047,0.063,0.017,0.052,0.084,0.019,0.018,0.056,0.040μg/L.

关 键 词：双硫腙复合凹凸棒土 重金属离子 固相萃取 电感耦合等离子体质谱法 

分 类 号：O65[理学—分析化学]