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首页> 美国卫生研究院文献>The Journal of Automatic Chemistry >A Method to Determination of Lead Ions in Aqueous Samples: Ultrasound-Assisted Dispersive Liquid-Liquid Microextraction Method Based on Solidification of Floating Organic Drop and Back-Extraction Followed by FAAS
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A Method to Determination of Lead Ions in Aqueous Samples: Ultrasound-Assisted Dispersive Liquid-Liquid Microextraction Method Based on Solidification of Floating Organic Drop and Back-Extraction Followed by FAAS

机译：一种测定水中样品中铅离子的方法：基于漂浮有机液滴固化和反萃取-FAAS的超声辅助分散液-液微萃取法

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Ultrasound-assisted dispersive liquid-liquid microextraction method based on solidification of floating organic drop and back-extraction (UA-DLLME-SFO-BE) technique was proposed for preconcentration of lead ions. In this technique, two SFODME steps are applied in sequence. The classical SFODME was applied as the first step and then the second (back-extraction) step was applied. For the classical SFODME, Pb ions were complexed with Congo red at pH 10.0 and then extracted into 1-dodecanol. After this stage, a second extraction step was performed instead of direct determination of the analyte ion in the classical method. For this purpose, the organic phase containing the extracted analyte ions is treated with 1.0 mol·L−1 HNO3 solution and then exposed to ultrasonication. So, the analyte ions were back-extracted into the aqueous phase. Finally, the analyte ions in the aqueous phase were determined by FAAS directly. Owing to the second extraction step, a clogging problem caused by 1-dodecanol during FAAS determination was avoided. Some parameters which affect the extraction efficiency such as pH, volume of extraction solvent, concentration of complexing agent, type, volume, and concentration of back-extraction solvent, effect of cationic surfactant addition, effect of temperature, and so on were examined. Performed experiments showed that optimum pH was 10.0, 1-dodecanol extraction solvent volume was 75 μL, back-extraction solvent was 500 μL, 1.0 mol·L−1 HNO3, extraction time was 4 min, and extraction temperature was 40°C. Under optimum conditions, the enhancement factor, limit of detection, limit of quantification, and relative standard deviation were calculated as 81, 1.9 μg·L−1, 6.4 μg·L−1, and 3.4% (for 25 μg·L−1 Pb2+), respectively.
机译：提出了一种基于漂浮有机液滴固化和反萃取的超声辅助分散液-液微萃取方法（UA-DLLME-SFO-BE）对铅离子进行预浓缩。在此技术中，依次执行两个SFODME步骤。第一步是应用经典的SFODME，然后是第二步（反萃取）。对于经典的SFODME，Pb离子与刚果红在pH 10.0处络合，然后萃取到1-十二烷醇中。在此阶段之后，执行第二步提取步骤，而不是采用传统方法直接测定分析物离子。为此，将含有提取的分析物离子的有机相用1.0？mol·L -1 HNO3溶液处理，然后进行超声处理。因此，将分析物离子反萃取到水相中。最后，通过FAAS直接测定水相中的分析物离子。由于第二提取步骤，避免了在FAAS测定过程中由1-十二烷醇引起的堵塞问题。研究了影响萃取效率的一些参数，例如pH，萃取溶剂的体积，络合剂的浓度，反萃取溶剂的类型，体积和浓度，阳离子表面活性剂添加的影响，温度的影响等。实验表明，最佳pH为10.0，1-十二烷醇萃取溶剂体积为75μL，反萃取溶剂为500μμL，1.0mol·L -1 HNO3，萃取时间为4 min，萃取温度为40℃。在最佳条件下，计算出增强因子，检出限，定量限和相对标准偏差为81、1.9μg·L -1 ，6.4μg·L -1 。 sup>和3.4％（对于25μg·L -1 Pb 2 + ）。

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