Sorouraddin Saeed Mohammad, Farajzadeh Mir Ali, Okhravi Tohid
Department of Analytical Chemistry, Faculty of Chemistry, University of Tabriz, Tabriz, Iran.
Department of Analytical Chemistry, Faculty of Chemistry, University of Tabriz, Tabriz, Iran; Engineering Faculty, Near East University, 99138 Nicosia, North Cyprus, Mersin 10, Turkey.
Talanta. 2017 Dec 1;175:359-365. doi: 10.1016/j.talanta.2017.07.065. Epub 2017 Jul 22.
A new sample preparation method has been developed for extraction and preconcentration of some heavy metal cations in aqueous samples using cyclohexylamine-based homogeneous liquid-liquid microextraction. In the proposed method, cyclohexylamine was used as both the complexing agent and the extraction solvent. For this purpose, cyclohexylamine at µL level was initially added into an aqueous solution containing Co(II), Ni(II), and Cu(II) ions which was placed in a glass test tube. The mixture was shaken for forming a homogeneous solution. Then sodium chloride was added to the solution. After shaking manually again, the test tube was placed in a water bath thermostated at 70°C. Due to lower solubility of cyclohexylamine at the elevated temperature, a cloudy solution was formed. The fine droplets of cyclohexylamine containing cation-cyclohexylamine complexes were collected on the top of the aqueous phase by centrifuging. The enriched analytes in the upper phase were determined by graphite furnace atomic absorption spectrometry. Several variables possibly affecting the extraction efficiency were investigated and optimized. Under the optimum conditions the calibration curves were linear in the ranges of 80-1000, 40-700, and 80-800ngL for Co, Ni, and Cu, respectively. Repeatability of the proposed method, expressed as relative standard deviation, ranged from 3.3% to 5.2% (n = 6, C = 200ngL). Moreover, the obtained detection limits of the selected analytes were in the range of 15.3-37.7ngL. The accuracy of the developed procedure was verified by analyzing a certified reference material, namely NRCC-SLRS4 Riverine water. Finally, the proposed method was successfully applied for the simultaneous analysis of the selected analytes in environmental water samples.
已开发出一种新的样品制备方法,用于使用环己胺基均相液 - 液微萃取法萃取和预富集水样中的一些重金属阳离子。在所提出的方法中,环己胺既用作络合剂又用作萃取溶剂。为此,首先将微升量的环己胺加入置于玻璃试管中的含有Co(II)、Ni(II)和Cu(II)离子的水溶液中。将混合物振荡以形成均匀溶液。然后向溶液中加入氯化钠。再次手动振荡后,将试管置于70°C的恒温水浴中。由于环己胺在升高温度下的溶解度降低,形成了浑浊溶液。通过离心在水相顶部收集含有阳离子 - 环己胺络合物的环己胺细液滴。通过石墨炉原子吸收光谱法测定上层相中富集的分析物。研究并优化了几个可能影响萃取效率的变量。在最佳条件下,Co、Ni和Cu的校准曲线分别在80 - 1000、40 - 700和80 - 800 ng/L范围内呈线性。所提出方法的重复性以相对标准偏差表示,范围为3.3%至5.2%(n = 6,C = 200 ng/L)。此外,所选分析物的检测限在15.3 - 37.7 ng/L范围内。通过分析一种有证标准物质,即NRCC - SLRS4河流水,验证了所开发方法的准确性。最后,所提出的方法成功应用于环境水样中所选分析物的同时分析。