【摘要】 采用水热法合成单斜相纺锤形纳米二氧化锆(ZrO2),建立单斜相纺锤形纳米ZrO2富集分离电感耦合等离子体质谱(ICP-MS)测定水中痕量Ba(Ⅱ)的方法。对Ba(Ⅱ)的检出限为0.007ng.mL-1,相对标准偏差为0.13%(n=11);系统的研究纳米ZrO2对Ba(Ⅱ)的最佳富集分离条件,在pH 10.0时,纳米ZrO2对Ba(Ⅱ)的吸附率可达99%以上,以2mL 0.5mol.L-1的HCl为洗脱剂,可定量洗脱纳米ZrO2上吸附的Ba(Ⅱ),洗脱率达98%以上;考察了纳米ZrO2对Ba(Ⅱ)的静态吸附容量为196.6μg.g-1、富集倍数可达250倍;通过再生实验、共存离子的影响以及与普通ZrO2的对比实验探讨了纳米ZrO2的性能,并将纳米ZrO2的富集分离性能应用于实际样品中Ba(Ⅱ)的分析,使用ICP-MS进行测定,结果满意。更多还原

【Abstract】 Monoclinic fusiform zirconium dioxide(ZrO2) nanoparticles were synthesized by hydrothermal method,a method was established based on monoclinic fusiform nanometer-sized ZrO2 enrichment separation,and trace barium in water was determined by inductively coupled plasma mass spectrometry(ICP-MS).The detection limit for Ba(Ⅱ) was 0.007 ng·mL-1,and the relative standard deviation was 0.13%(n=11).The optimal enrichment separation conditions of nanometer-sized ZrO2 for Ba(Ⅱ) were studied in detail,it was found that the percentage of adsorbed Ba(Ⅱ) was more than 99% under pH 10.0 and 2 mL 0.5 mol·L-1 HCl was sufficient for elution of Ba(Ⅱ) by more than 98%.The static adsorption capacity of ZrO2 to Ba(Ⅱ) was 196.6 μg·g-1 and enrichment factor was 250.Properties of nanometer-sized ZrO2 were discussed through regeneration experiment and effects of co-existing ions and contrast experiment to ordinary ZrO2,adsorption properties of nanometer-sized ZrO2 were applied to real samples in the analysis of Ba(Ⅱ) and the determination was carried out by ICP-MS with satisfactory results.更多还原