采用室温固相法合成球形立方相纳米CeO2,建立了纳米CeO2富集分离,ICP-M S同时测定痕量Pb(Ⅱ)和Cd(Ⅱ)的方法。在pH 7.0,10 mg CeO2,吸附15min后,纳米CeO2对Pb(Ⅱ),Cd(Ⅱ)的吸附率均可达100%;以2mL 0.05 mol/L HCl溶液为洗脱剂、洗脱20 min后,对Pb(Ⅱ)和Cd(Ⅱ)的洗脱率可分别达到98%和95%以上;纳米CeO2对Pb(Ⅱ),Cd(Ⅱ)的最大静态吸附容量分别为496.9μg/g和243.1μg/g,富集倍数均可达250倍,共存离子影响小。优化ICP-MS仪器工作条件,选择205Bi和115In为在线内标进行Pb(Ⅱ)和Cd(Ⅱ)的测定,检出限分别为1.7 pg/mL和9.2 pg/mL,RSD分别为4.8%和0.94%。方法应用于实际水样,回收率分别为Pb(Ⅱ)93.6%~106.4%,Cd(Ⅱ)96.2%~108.9%。
Spherical cubic phase cerium dioxide (CeO2 ) nanoparticles were synthesized through a solid-state reaction at room temperature. A method was established based on nanometer CeO2 enrichment of trace Pb ( Ⅱ ) and Cd ( Ⅱ ) and determination by inductively coupled plasma mass spectrometry ( ICP-MS ). Adsorption percentages of Pb( Ⅱ ) and Cd(Ⅱ ) up to 100% with nanometer CeO2 10 mg under pH 7.0 for 15 min, then 2 mL 0.05 mol/L HC1 were sufficient for more than 98% elution efficiency of Pb( Ⅱ ) and more than 95% elution efficiency of Cd ( Ⅱ ) within 20 min. static adsorption capacities of CeO2 to Pb ( Ⅱ ) and Cd ( Ⅱ ) were 496.9μg and 243. 0 μg/g with enrichment factors reaching to 250, little effects of co-existing ions. Optimization of ICP-MS working conditions, 205Bi and 115In as online internal standard elements for determination, detection limits for Pb( Ⅱ ) and Cd( Ⅱ ) were 1.7 and 9.2 pg/mL, relative standard deviations were 4.8% and 0.94%, respectively. The method had been applied to real water samples, recoveries of Pb( Ⅱ ) and Cd( Ⅱ ) were 93.6% ~ 106. 4% and 96. 2% - 108.9% with satisfactory results.