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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%。
The spherical cubic nanocrystalline CeO2 was synthesized by solid state reaction at room temperature. The method for the simultaneous determination of trace amounts of Pb (Ⅱ) and Cd (Ⅱ) by ICP-MS was established. The adsorption rates of Pb (Ⅱ) and Cd (Ⅱ) by nanometer CeO2 can reach 100% at pH 7.0, 10 mg CeO2 and 15 min after adsorption, respectively. When 2 mL 0.05 mol / L HCl solution is used as eluent, , The elution rates of Pb (Ⅱ) and Cd (Ⅱ) reached 98% and 95%, respectively. The maximum static adsorption capacity of CeO2 to Pb (Ⅱ) and Cd (Ⅱ) was 496.9μg / g and 243.1μg / g, enrichment fold up to 250 times, the impact of coexisting ions is small. The detection limits of Pb (Ⅱ) and Cd (Ⅱ) were determined by on-line internal standard with the detection limits of 1.7 pg / mL and 9.2 pg / mL, and the RSDs were 4.8% and 0.94%. The method was applied to the actual water samples. The recoveries were 93.6% -106.4% for Pb (Ⅱ) and 96.2% -108.9% for Cd (Ⅱ) respectively.