球形立方相纳米二氧化铈-ICP-MS法同时测定痕量铅和镉  

Simultaneous determination of trace lead and cadmium with spherical cubic phase CeO_2 nanoparticles preconcentration and ICP-MS

作　　者：杜英秋[1,2] 

机构地区：[1]黑龙江省农业科学院农产品质量安全研究所,哈尔滨150086 [2]黑龙江大学化学化工与材料学院,哈尔滨150080

出　　处：《分析试验室》2015年第5期515-519,共5页Chinese Journal of Analysis Laboratory

基　　金：国家自然科学基金项目(20871043)资助

摘　　要：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.

关 键 词：纳米二氧化铈 ICP-MS 铅 镉 

分 类 号：O657.63[理学—分析化学]