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Dispersive liquid–liquid micro extraction of uranium(VI) from groundwater and seawater samples and determination by inductively coupled plasma–optical emission spectrometry and flow injection–inductively coupled plasma mass spectrometry

机译:从地下水和海水样品中进行液-液微萃取铀(VI),并通过电感耦合等离子体发射光谱法和流动注射电感耦合等离子体质谱法测定

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A dispersive liquid–liquid microextraction (DLLME) method was developed for the determination of uranium(VI) in groundwater/seawater by inductively coupled plasma–optical emission spectrometry (ICP–OES) and flow injection–inductively coupled plasma mass spectrometry (FI–ICPMS). This is the first report on the extraction of uranium(VI) by a DLLME method. In this method, uranium(VI) was complexed with ammonium pyrrolidine dithiocarbamate (APDC) in the presence of cetyltrimethyl ammonium bromide (CTAB), which enhanced the hydrophobicity of the ion–association complex resulting in improved extraction into chloroform. The extraction was carried out after adjusting the pH of the water sample to 1. The uranyl ion was back extracted from chloroform layer with nitric acid for determination by ICP–OES/FI–ICPMS. Some effective parameters for complex formation and extraction, such as volume of extraction and disperser solvent, extraction time, pH and concentration of the chelating agent and surfactant have been optimized using ICP–OES. Under optimum conditions, enrichment factors of 11 and 25 were obtained from 10 mL of water sample for determinations by ICP–OES and FI–ICPMS respectively. The calibration graphs were linear in the range of 5–200 μg L?1 and 50–5000 ng L?1 with limits of detection of 2.0 μg L?1 and 30 ng L?1 respectively for ICP–OES and FI–ICPMS. The method has been applied to a few groundwater and seawater samples. The recoveries obtained for uranium(VI) in groundwater and seawater samples spiked to levels of 10 and 5 μg L?1 were 90–105% respectively. The results obtained by the proposed method have been cross validated by laser fluorimetry...
机译:开发了一种分散液-液微萃取(DLLME)方法,用于通过电感耦合等离子体发射光谱法(ICP-OES)和流动注射电感耦合等离子体质谱法(FI-ICPMS)测定地下水/海水中的铀(VI) )。这是关于通过DLLME方法提取铀(VI)的第一份报告。在这种方法中,在十六烷基三甲基溴化铵(CTAB)存在下,将铀(VI)与吡咯烷二硫代氨基甲酸铵(APDC)络合,这增强了离子缔合复合物的疏水性,从而改善了对氯仿的萃取。在将水样品的pH值调整为1之后进行萃取。用硝酸从氯仿层中反萃取铀酰离子,以通过ICP-OES / FI-ICPMS测定。 ICP-OES已优化了一些复杂的形成和萃取有效参数,例如萃取和分散剂的体积,萃取时间,pH值以及螯合剂和表面活性剂的浓度。在最佳条件下,从10 mL水样品中分别获得11和25的富集系数,分别通过ICP-OES和FI-ICPMS测定。校准曲线在5–200μgL?1和50–5000 ng L?1范围内是线性的,对于ICP–OES和FI–ICPMS,检出限分别为2.0μgL?1和30 ng L?1。该方法已应用于一些地下水和海水样品。掺入10和5μgL?1的地下水和海水样品中铀(VI)的回收率分别为90–105%。所提出的方法获得的结果已通过激光荧光法交叉验证。

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