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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。
Hydrothermal synthesis of monoclinic spindle-shaped nanosized zirconia (ZrO2), the establishment of monoclinic spindle-shaped nanometer ZrO2 enrichment separation inductively coupled plasma mass spectrometry (ICP-MS) method for the determination of trace Ba (Ⅱ) in water. The detection limit of Ba (Ⅱ) was 0.007ng.mL-1, with a relative standard deviation of 0.13% (n = 11). The optimal conditions for the enrichment and separation of Ba (Ⅱ) , The adsorption rate of Ba (Ⅱ) to nano-ZrO2 can reach more than 99%. The amount of Ba (Ⅱ) adsorbed on nano-ZrO2 can be quantitatively eluted with 2mL 0.5mol.L-1 HCl as eluent, Up to 98%. The static adsorption capacity of nano-ZrO2 for Ba (Ⅱ) was 196.6μg.g-1 and the enrichment factor was up to 250 times. The effects of coexisting ions and the comparison with ordinary ZrO2 The performance of nano-ZrO2 was studied. The enrichment and separation of nano-ZrO2 was applied to the analysis of Ba (Ⅱ) in real samples. The results were satisfactory with ICP-MS.