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Analysis of trace mercury in water by solid phase extraction using dithizone modified nanometer titanium dioxide and cold vapor atomic absorption spectrometry

机译:双硫zone修饰纳米二氧化钛固相萃取-冷原子吸收光谱法测定水中痕量汞。

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摘要

A new method for analysis of trace mercury in water samples was developed, based on the combination of preconcentration/separation using dithizone-modified nanometer titanium dioxide (TiO_2) as a solid phase extractant and determination by cold vapor atomic adsorption spectrometry (CVAAS). Dithizone was dissolved with alcohol and loaded on the surface of nano-sized TiO_2 powders by stirring. The static adsorption behavior of Hg~(2+)on the dithizone-modified nanoparticles was investigated in detail. It was found that excellent adsorption ratio for Hg~(2+) could be obtained in the pH range of 7-8 with an oscillation time of 15 min, and a 5 mL of 3.5 mol·L~(-1) HC1 solution could quantitatively elute Hg~(2+) from nanometer TiO_2 powder. Common coexisting ions caused no obvious influence on the determination of mercury. The mechanisms for the adsorption and desorption were discussed. The detection limit (3σ) for Hg~(2+) was calculated to be 5 ng·L~(-1). The proposed method was applied to the determination of Hg~(2+) in a mineral water sample and a Zhujiang River water sample. By the standard addition method, the average recoveries were found to be 94.4%-108.3% with RSD (n = 5) of 2.9%-3.5%.
机译:基于双硫zone改性纳米二氧化钛(TiO_2)作为固相萃取剂的预浓缩/分离与冷蒸气原子吸收光谱法(CVAAS)的结合,开发了一种用于分析水中痕量汞的新方法。将双硫zone溶于乙醇,并通过搅拌将其负载在纳米TiO_2粉末的表面上。详细研究了Hg〜(2+)在双硫zone改性纳米颗粒上的静态吸附行为。结果表明,在pH值为7〜8,振荡时间为15 min的条件下,对Hg〜(2+)的吸附率较高,在5 mol的3.5mol·L〜(-1)HCl溶液中,Hg〜(2+)的吸附率最高。从纳米TiO_2粉末中定量洗脱出Hg〜(2+)。常见的共存离子对汞的测定没有明显影响。讨论了吸附和解吸的机理。 Hg〜(2+)的检出限(3σ)经计算为5 ng·L〜(-1)。该方法用于矿泉水和珠江水样中Hg〜(2+)的测定。通过标准添加方法,发现平均回收率为94.4%-108.3%,RSD(n = 5)为2.9%-3.5%。

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