Study on the Method of Nanometer-Size Zirconium Dioxide Enrichment Separation and Inductively Coupled Plasma Mass Spectrometry Determination of Trace Barium(Ⅱ) in Water
DU Ying-qiu1, 2, YIN Yi-dong1*, FAN Nai-ying1, CHEN Peng-gang1, ZHANG Xiao-bo2, REN Hong-bo2, CHEN Guo-you2, QU Qiu-yao1, SUN Zhi-bo1, CHEN Yue-xin1
1. School of Chemical Engineering & Materials, Heilongjiang University, Harbin 150080, China 2. Inspection and Testing Center for Quality of Cereals and Their Products(Harbin), Ministry of Agriculture, Harbin 150086, China
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0.007 ng·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2 mL 0.5 mol·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196.6 μg·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。
关键词：纳米二氧化锆;富集;分离;ICP-MS;钡
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.
杜英秋1, 2，尹贻东1*，范乃英1，陈鹏刚1，张晓波2，任红波2，陈国友2，屈秋瑶1，孙智博1，陈月鑫1. 纳米二氧化锆富集分离电感耦合等离子体质谱测定水中痕量钡(Ⅱ)的方法研究[J]. 光谱学与光谱分析, 2012, 32(11): 3129-3134.
DU Ying-qiu1, 2, YIN Yi-dong1*, FAN Nai-ying1, CHEN Peng-gang1, ZHANG Xiao-bo2, REN Hong-bo2, CHEN Guo-you2, QU Qiu-yao1, SUN Zhi-bo1, CHEN Yue-xin1 . Study on the Method of Nanometer-Size Zirconium Dioxide Enrichment Separation and Inductively Coupled Plasma Mass Spectrometry Determination of Trace Barium(Ⅱ) in Water. SPECTROSCOPY AND SPECTRAL ANALYSIS, 2012, 32(11): 3129-3134.
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