本文制备了磁性固相萃取材料Fe_3O_4@ILs-β-CDCP,并对其进行了表征。详细考察了Fe_3O_4@ILs-β-CDCP萃取Pb(Ⅱ)和Sb(Ⅲ)的各种影响因素,如溶液pH值、样品体积、洗脱剂浓度和用量、洗脱剂类型、共存离子影响等。基于此,建立了磁固相萃取-电感耦合等离子体发射光谱法(ICP-OES)同时测定Pb(Ⅱ)和Sb(Ⅲ)的新方法。在优化的条件下,该方法对Pb(Ⅱ)和Sb(Ⅲ)的检出限分别为1.50和0.54ng/mL,相对标准偏差(RSDs)分别为5.9%和2.4%(n=6,c=100.0ng/mL)。将该方法应用于实际水样中Pb(Ⅱ)和Sb(Ⅲ)的测定,其回收率分别为77.8%~106%和82.4%~107%。方法具有检出限低、操作简便等优势。
Magnetic solid phase extraction coupled with ICP-OES for the simultaneous determination of Pb(Ⅱ)and Sb(Ⅱ)was developed.This method based on the fact that Fe_3O_4@ILs-β-CDCP polymer could be employed as an absorbent.The factors affecting separation and preconcentration of target analytes such as pH,sample volume,eluent concentration and volume,interfering ions were investigated.Under the optimized conditions,the detection limits for Pb(Ⅱ)and Sb(Ⅲ)were 1.50 and 0.47ng/mL,and the relative standard deviations were 5.9% and 2.4%(n=6,c=100.0ng/mL),respectively.The proposed method was successfully applied to determine Pb(Ⅱ)and Sb(Ⅲ)in real water samples with recovery of 82.41%-106.8% and 77.84%-106.1%,respectively.