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    高效液相色谱-电感耦合等离子体质谱法测定淡水中7种元素形态的含量

    HPLC-ICP-MS Determination of 7 Element Species in Fresh Water

    • 摘要: 建立了高效液相色谱-电感耦合等离子体质谱法同时测定淡水中亚砷酸盐As(Ⅲ)、砷酸盐As(Ⅴ)、一甲基胂酸(MMA)、二甲基胂酸(DMA)、亚硒酸盐Se(Ⅳ)、硒酸盐Se(Ⅵ)和六价铬Cr(Ⅵ)的方法。采用以不同体积比的pH 8.7的20 mmol·L-1硝酸铵溶液和pH 8.7的60 mmol·L-1硝酸铵溶液为流动相进行梯度洗脱,通过优化的色谱条件实现了7种元素形态在14 min完成色谱分离,氯化物对75As、77Se、53Cr无干扰。7种元素形态在一定范围内呈线性,As(Ⅲ)、As(Ⅴ)、MMA、DMA、Se(Ⅳ)、Se(Ⅵ)和Cr(Ⅵ)的检出限(3S/N)分别为0.06,0.02,0.04,0.05,1.00,1.00,0.20 μg·L-1。按标准加入法进行回收试验,回收率为80.1%~101%,相对标准偏差(n=6)为0.59%~5.2%。

       

      Abstract: A method was proposed for simultaneous determination of arseniteAs(Ⅲ), arsenateAs(Ⅴ), monomethylarsenic acid (MMA), dimethylarsenic acid (DMA), seleniteSe(Ⅳ), selenateSe(Ⅵ) and Cr(Ⅵ) in fresh water by high performance liquid chromatography-inductively coupled plasma-mass spectrometry (HPLC-ICP-MS). A mixture of 20 mmol·L-1 NH4NO3 solution (pH 8.7) and 60 mmol·L-1 NH4NO3 solution (pH 8.7) in different volume ratios was used as the mobile phase for gradient elution. Seven element species were separated under the optimized chromatographic conditions within 14 min, and the chloride had no interference to 75As, 77Se and 53Cr. Linear relationships of 7 element species were found in definite ranges, and the detection limits were 0.06 μg·L-1 for As (Ⅲ), 0.02 μg·L-1 for As(Ⅴ), 0.04 μg·L-1 for MMA, 0.05 μg·L-1 for DMA, 1.00 μg·L-1 for Se(Ⅳ), 1.00 μg·L-1 for Se(Ⅵ) and 0.20 μg·L-1 for Cr(Ⅵ), respectively. Test for recovery was made by standard addition method, giving results in the range of 80.1%-101%, with RSDs (n=6) ranged from 0.59% to 5.2%.

       

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