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基于固化漂浮有机滴的超声辅助乳化微萃取用于石墨炉原子吸收光谱法测定痕量锰之前的样品处理

Ultrasound-assisted emulsification microextraction based on solidification floating organic drop trace amounts of manganese prior to graphite furnace atomic absorption spectrometry determination.

作者信息

Mohadesi Alireza, Falahnejad Masoumeh

机构信息

Department of Chemistry, Payame Noor University, PO Box 19395-3697, Tehran, Iran. mohadesi

出版信息

ScientificWorldJournal. 2012;2012:987645. doi: 10.1100/2012/987645. Epub 2012 May 2.

Abstract

In the present study, an ultrasound-assisted emulsification microextraction based on solidification floating organic drop method is described for preconcentration of trace amounts of Mn (II). 2-(5-Bromo-2-pyridylazo)-5 diethylaminophenol was added to a solution of Mn(+2) at ph = 10.0. After this, 1-undecanol was added to the solution as an extraction solvent, and solution was stirred. Several factors influencing the microextraction efficiency, such as pH, the amount of chelating agent, nature and volume of extraction solvent, the volume of sample solution, stirring rate, and extraction time were investigated and optimized. Then sample vial was cooled by inserting into an ice bath, and the solidified was transferred into a suitable vial for immediate melting. Finally the sample was injected into a graphite furnace atomic absorption spectrometry. Under the optimum condition the linear dynamic range was 0.50-10.0 ng mL(-1) with a correlation coefficient of 0.9926, and the detection limit of 0.3 ng mL(-1) was obtained. The enrichment factor was 160. The proposed method was successfully applied for separation and determination of manganese in sea, rain, tap, and river water samples.

摘要

在本研究中,描述了一种基于固化漂浮有机滴法的超声辅助乳化微萃取方法,用于痕量锰(II)的预富集。在pH = 10.0的锰(+2)溶液中加入2-(5-溴-2-吡啶偶氮)-5-二乙氨基苯酚。此后,向溶液中加入1-十一醇作为萃取溶剂,并搅拌溶液。研究并优化了影响微萃取效率的几个因素,如pH值、螯合剂用量、萃取溶剂的性质和体积、样品溶液体积、搅拌速率和萃取时间。然后将样品瓶插入冰浴中冷却,将固化物转移到合适的样品瓶中立即熔化。最后将样品注入石墨炉原子吸收光谱仪中。在最佳条件下,线性动态范围为0.50 - 10.0 ng mL(-1),相关系数为0.9926,检测限为0.3 ng mL(-1)。富集因子为160。该方法成功应用于海水、雨水、自来水和河水样品中锰的分离和测定。

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