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首页> 外文期刊>Mikrochimica Acta: An International Journal for Physical and Chemical Methods of Analysis >Determination of trace mercury in environmental samples by cold vapor atomic fluorescence spectrometry after cloud point extraction
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Determination of trace mercury in environmental samples by cold vapor atomic fluorescence spectrometry after cloud point extraction

机译:浊点萃取后冷蒸气原子荧光光谱法测定环境样品中的痕量汞

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摘要

A sensitive method is presented for the determination of ultra-trace levels of mercury using cold vapor atomic fluorescence spectrometry along with cloud point extraction. Preconcentration is based on the complexation of Hg(II) by dithizone, followed by micelle-mediated extraction of the complex using the surfactant Triton X-l 14. Foaming, which is always observed when generating vapor mercury in the presence of surfactant, was strongly reduced by using SnCl2 as a reducing reagent, and a homemade gas-liquid separator. Variables that affect the assay were optimized. These included pH value, concentration of chelating reagent, concentration of Triton X-114, equilibration temperature and time. The preconcentration of a 45-mL sample gave an enhancement factor of 29. The calibration graph is linear in the range from 0.05 to 5.0 ngmL~(-1) with a correlation coefficient of 0.9991. The limit of detection (36) obtained under the optimal conditions is 5 pgmL~(-1). The relative standard deviation for seven replicate determinations at 0.5 ngmL~(-1) level is 5.2%. The method was successfully applied to the determination of Hg in real samples.
机译:提出了一种灵敏的方法,用于使用冷蒸气原子荧光光谱法和浊点萃取法测定痕量汞。预浓缩基于双硫zone对Hg(II)的络合,然后使用表面活性剂Triton Xl 14进行胶束介导的络合物萃取。通过在表面活性剂的存在下生成蒸气汞时经常观察到的泡沫现象可以大大减少使用SnCl2作为还原剂和自制的气液分离器。优化了影响测定的变量。其中包括pH值,螯合剂浓度,Triton X-114浓度,平衡温度和时间。预浓缩的45 mL样品的增强因子为29。校正图在0.05至5.0 ngmL〜(-1)范围内呈线性关系,相关系数为0.9991。在最佳条件下获得的检出限(36)为5 pgmL〜(-1)。在ngmL〜(-1)浓度下进行7次重复测定的相对标准偏差为5.2%。该方法已成功应用于实际样品中汞的测定。

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