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表面活性剂辅助分散液液微萃取法与中心复合设计在基于微体积分光光度法测定水样品中低水平六价铬离子中的应用。

Application of a surfactant-assisted dispersive liquid-liquid microextraction method along with central composite design for micro-volume based spectrophotometric determination of low level of Cr(VI) ions in aquatic samples.

机构信息

Department of Chemistry, Payame Noor University, Tehran, Iran.

Department of Chemistry, Payame Noor University, Tehran, Iran.

出版信息

Spectrochim Acta A Mol Biomol Spectrosc. 2018 Sep 5;202:36-40. doi: 10.1016/j.saa.2018.05.031. Epub 2018 May 9.

Abstract

A fast, simple, low cost surfactant-assisted dispersive liquid-liquid microextraction method along with central composite design for the determination of low level of Cr(VI) ions in several aquatic samples has been developed. Initially, Cr(VI) ions present in the aqueous sample were readily reacted with 1,5‑diphenylcarbazide (DPC) in acidic medium through complexation. Sodium dodecyl sulfate (SDS), as an anionic surfactant, was then employed as an ion-pair agent to convert the cationic complex into the neutral one. Following on, the whole aqueous phase underwent a dispersive liquid-liquid microextraction (DLLME) leading to the transfer of the neutral complex into the fine droplet of organic extraction phase. A micro-volume spectrophotometer was used to determine Cr(VI) concentrations. Under the optimized conditions predicted by the statistical design, the limit of quantification (LOQ) obtained was reported to be 5.0 μg/L, and the calibration curve was linear over the concentration range of 5-100 μg/L. Finally, the method was successfully implemented for the determination of low levels of Cr(VI) ions in various real aquatic samples and the accuracies fell within the range of 83-102%, while the precision varied in the span of 1.7-5.2%.

摘要

建立了一种快速、简单、低成本的表面活性剂辅助分散液液微萃取方法,并结合中心复合设计,用于测定几种水样中的低水平六价铬离子。首先,水样中的六价铬离子在酸性介质中与 1,5-二苯基卡巴肼(DPC)迅速反应,通过络合形成络合物。然后,十二烷基硫酸钠(SDS)作为阴离子表面活性剂,用作离子对试剂,将阳离子络合物转化为中性络合物。接着,整个水相经历分散液液微萃取(DLLME),将中性络合物转移到有机萃取相的细小液滴中。使用微体积分光光度计测定 Cr(VI)浓度。在统计设计预测的最佳条件下,得到的检出限(LOQ)为 5.0μg/L,校准曲线在 5-100μg/L 的浓度范围内呈线性。最后,该方法成功用于各种实际水样中低水平六价铬离子的测定,其准确度在 83-102%范围内,而精密度在 1.7-5.2%范围内变化。

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