| 摘要: |
| 采用氢化物-原子荧光光度法(HG-AFS), 测定天然水体中的总溶解态无机锑(Sb(Ⅴ+III))和三价锑(Sb(III))。选择的最佳仪器条件为: 灯电流60 mA, 负高压?260 V, 原子化器的温度190 ℃和氩气的载气流量600 mL/min。Sb(Ⅴ+III)在1 mol/L HCl 介质中进行测定, 检出限为0.024 μg/L, 线性范围为0～14 μg/L。对浓度0.3 μg/L 和0.03 μg/L 的样品分析精密度分别为2.0% 和1.9%(n=9), 方法的回收率93.7%～105%。Sb(III)是在柠檬酸和柠檬酸钠缓冲溶液中(pH 为4.0～4.5), 辅以100 mL/min 的氢气进行测定,测得检出限为0.0013 μg/L, 对浓度0.04 μg/L 和0.01 μg/L 的样品分析精密度分别为3.8% 和5.5%(n=9), 方法的回收率91.1%～104%。二者在不同介质中工作曲线的斜率变动范围均小于5%。Sb(Ⅴ)的含量由总溶解态无机锑与三价锑的含量差减得到。 |
| 关键词: 原子荧光光度法 Sb(V) Sb(III) 天然水体 |
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| 基金项目:国家重点基础研究发展规划项目(2006CB400601); 国家自然科学青年基金项目(40606028) |
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| Determination of major antimony species (Sb(V) and Sb(III)) in natural water by hydride generation atomic fluorescence spectrometry |
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| Abstract: |
| A method for the determination of Sb (Ⅴ+III) and Sb (III) by atomic fluorescence spectrometry (AFS) in natural water was established in this study. The optimal instrumental parameters were electric current, 60 mA; voltage, ?260 V; temperature, 190 ℃; and Ar flux, 600 mL/min. The method was based on the behavior of total antimony (Sb(V+III)) and antimony (III) under different acidic conditions. Total antimony was determined at 1 mol/L HCl; and antimony (III) was determined at pH =4.0～4.5. Under optimized conditions, the detection limit (3σ) for Sb (V+III) and Sb(III) were 0.024 μg/L and 0.0013 μg/L, respectively. For total antimony, the precision for the sample of 0.3 μg/L or 0.03 μg/L was 1.95% or 1.92%, respectively (n= 9). The linearity was 0～14 μg/L. For antimony (III), the precision for the sample of 0.04 μg/L or 0.01 μg/L are 3.8% or 5.5%, respectively (n = 9). The recoveries for Sb(Ⅴ+III) and Sb(III) are 93.7%~105% and 91.1%~104%, respectively. The method can be used directly to the determination of Sb (V+III) and Sb (III) in natural water. |
| Key words: Atomic fluorescence spectrometry Sb(V) Sb(III) natural water |
