Eftekhari Mohammad, Chamsaz Mahmoud, Arbab-Zavar Mohammad Hossein, Eftekhari Ali
Department of Chemistry, Ferdowsi University of Mashhad, Mashhad, Iran,
Environ Monit Assess. 2015 Jan;187(1):4129. doi: 10.1007/s10661-014-4129-3. Epub 2014 Nov 18.
Vortex-assisted surfactant-enhanced emulsification microextraction based on solidification of floating organic drop (VASEME-SFO) was used for preconcentration and speciation of antimony (ΙΙΙ, V) followed by electrothermal atomic absorption spectrometry (ETAAS). In this procedure, Triton X-114 was used as emulsifier and 1-undecanol was used as extraction solvent. This method is based on the complexation of Sb(ΙΙΙ) with dithizone (as complexing agent) at pH 2 and extraction of the resulting hydrophobic complex into the extraction solvent (1-undecanol) with vortex-assisted liquid phase microextraction, whereas Sb(V) remained in solution. Sb(ΙΙΙ) in extraction solvent was directly analyzed by ETAAS after dilution with ethanol, and Sb(V) was calculated by subtracting Sb(ΙΙΙ) from the total antimony after reducing Sb(V) to Sb(ΙΙΙ) by L-cysteine. Under the optimized condition, the calibration curve was linear in the range of 0.4-8 μg L(-1) of Sb(ΙΙΙ) with a correlation coefficient of 0.9995. The detection limit based on three times of the standard deviation of the blank (n = 8) was 0.09 μg L(-1). The validation and the recovery of the proposed method were performed by the analysis of a certified reference material and spike method. The obtained results were in very good agreements with certified values. The proposed method was successfully applied for the determination of antimony species at trace levels in different water samples.
基于漂浮有机滴固化的涡旋辅助表面活性剂增强乳化微萃取法(VASEME-SFO)用于锑(III、V)的预富集和形态分析,随后采用电热原子吸收光谱法(ETAAS)进行测定。在此过程中,Triton X-114用作乳化剂,1-十一醇用作萃取溶剂。该方法基于在pH 2条件下Sb(III)与双硫腙(作为络合剂)的络合反应,通过涡旋辅助液相微萃取将生成的疏水络合物萃取到萃取溶剂(1-十一醇)中,而Sb(V)则保留在溶液中。萃取溶剂中的Sb(III)用乙醇稀释后直接通过ETAAS分析,Sb(V)通过用L-半胱氨酸将Sb(V)还原为Sb(III)后,从总锑中减去Sb(III)来计算。在优化条件下,Sb(III)的校准曲线在0.4 - 8 μg L⁻¹范围内呈线性,相关系数为0.9995。基于空白标准偏差的三倍(n = 8)的检测限为0.09 μg L⁻¹。通过分析有证标准物质和加标法对所提出方法进行了验证和回收率测定。获得的结果与认证值非常吻合。所提出的方法成功应用于不同水样中痕量锑形态的测定。