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采用双水相微乳液体系萃取和预富集,结合高分辨连续光源原子吸收光谱法测定痕量重金属的新方法。

A new method for extraction and pre-concentration of the heavy metals using a microemulsion system in winsor II equilibrium and determination by HR-CS AAS.

机构信息

Instituto de Química, Universidade Federal do Rio Grande do Norte, Núcleo de Processamento Primário e Reuso de Água Produzida, NUPPRAR, 59078-970, Natal, Brazil.

Instituto de Química, Universidade Federal do Rio Grande do Norte, Núcleo de Processamento Primário e Reuso de Água Produzida, NUPPRAR, 59078-970, Natal, Brazil.

出版信息

Chemosphere. 2023 Oct;338:139428. doi: 10.1016/j.chemosphere.2023.139428. Epub 2023 Jul 10.

Abstract

For the very first time, a microemulsion system in the Winsor II (WII) equilibrium was applied in a sample preparation method for extraction and pre-concentration in the determination of Pb, Cd, Co, Tl, Cu and Ni, in natural waters by high resolution continuum source atomic absorption spectrometry (HR-CS AAS). The method was optimized using the graphite furnace atomization. A simplex-centroid design for determine optimum extraction condition (77.5% aqueous phase, 5% of the oil phase, and 17.5% cosurfactant/surfactant ratio - C/S = 4) was applied. The optimized time for the sample preparations was around 30 min. The analytical performance of the optimized method using HR-CS GF AAS showed that the detection limits were: 0.09, 0.01, 0.06, and 0.05 μg L for determination of Pb, Cd, Tl, and Co, respectively and the enrichment factors were between 6 and 19, considered excellent for all analytes. The RSD values were lower than 5%, demonstrating the good precision of the proposed method. When the optimized method was applied using the HR-CS F AAS, the sensibility increased 9 to 12 times for Cu and Ni, respectively. The analytical method was successfully applied for the determination of analytes in Certified Reference Material and real samples for natural waters such as Brackish water (recovery between 107 and 112%), Saline water (recovery between 83 and 94%), Produced water from oil industry (recovery between 98 and 110%) and Fresh water (recovery 80 and 87% to Cu and Ni respectively). All the results confirming the accuracy of the analytical method proposed. The repeatability of the measurements has been better 5% (n = 3), for all elements.

摘要

首次将 Winsor II(WII)平衡中的微乳液体系应用于一种样品制备方法,用于通过高分辨率连续光源原子吸收光谱法(HR-CS AAS)在天然水中萃取和预浓缩 Pb、Cd、Co、Tl、Cu 和 Ni。该方法通过石墨炉原子化进行了优化。采用单纯形质心法设计来确定最佳萃取条件(77.5%水相、5%油相和 17.5%助表面活性剂/表面活性剂比-C/S=4)。样品制备的最佳时间约为 30 分钟。使用 HR-CS GF AAS 对优化方法的分析性能进行了研究,结果表明,Pb、Cd、Tl 和 Co 的检测限分别为 0.09、0.01、0.06 和 0.05μg/L,富集因子在 6 到 19 之间,对于所有分析物均认为是优异的。RSD 值低于 5%,表明该方法具有良好的精密度。当使用 HR-CS F AAS 应用优化方法时,Cu 和 Ni 的灵敏度分别提高了 9 到 12 倍。该分析方法成功应用于测定盐度水(回收率在 83%和 94%之间)、海水(回收率在 107%和 112%之间)、采油工业(回收率在 98%和 110%之间)和淡水(回收率分别为 80%和 87%)等天然水中的参考物质和实际样品中的分析物。所有结果都证实了所提出的分析方法的准确性。所有元素的测量重复性均优于 5%(n=3)。

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