Synthesis and modification of mercapto-submicron scavenger for real-time extraction and preconcentration of As(iii),Analytical Methods

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Synthesis and modification of mercapto-submicron scavenger for real-time extraction and preconcentration of As(iii)
Analytical Methods ( IF 2.7 ) Pub Date : 2017-12-20 00:00:00 , DOI: 10.1039/c7ay02490h
Nezar H. Khdary _{1,

2,

3} , Ahmed E. H. Gassim _{3,

4,

5,

6} , Alan G. Howard _{7,

8,

9,

10} , Tamil S. Sakthivel _{11,

12,

13,

14,

15} , Sudipta Seal _{11,

12,

13,

14,

15}

Affiliation

The gradual increase of arsenic in aquatic layers over the last decades has necessitated the early detection of low levels of arsenic on real time due to its hazardous impact on health. Here, the mercapto-submicron scavenger was synthesized and utilized for solid-phase dispersion extraction technique for real-time extraction and preconcentration of arsenite As(III). Because of particle size, they naturally dispersed without the need for any additional power. The formation of particles and the achievement of the modification of the particles were confirmed by SEM, TEM, size distributions, CHN analysis, FT-IR spectroscopy, micro-Raman spectroscopy, X-ray photoelectron spectroscopy (XPS), zeta potential, energy dispersive X-ray analysis and (EDX) and thermogravimetric analysis (TGA), which confirmed the formation of particles in the size of 253 ± 34 nm, the chemical implantation of the mercapto groups on the surface was successfully accomplished with a loading of 0.281 mmol g⁻¹. The particles showed proper dispersion and stability in the aqueous phase before and after being associated with As(III). The chelating process between As(III) and mercapto groups was assessed by XPS which confirmed that the mercapto-submicron scavenger can sequestrate As(III) from water with maximum efficiency. Several factors that could optimize the process were assessed such as the effect of sorbent dose, pH, contact time, sample volumes, eluents, and matrix interference. The As(III) calibration curve showed a positive linear correlation in the range of 0–100 μg L⁻¹ and coefficient of determination (r² = 0.9981). Optimum recovery was obtained with an equilibrium time of 30 min at pH = 8.5. It was found that the release of As(III) from the mercapto-submicron scavenger was eluent dependent and the maximum recovery at the optimum conditions was 98 ± 3%. The average recovery of As(III) from three different ground water locations was 97.15%.

中文翻译：

巯基亚微米清除剂的合成和修饰，用于实时提取和预富集As（iii）

在过去的几十年中，水层中砷的逐渐增加，由于其对健康的有害影响，必须实时地及早发现低水平的砷。在这里，合成了巯基-亚微米清除剂，并用于固相分散萃取技术中，实时提取和预富集砷（III）。）。由于粒径的原因，它们自然分散而无需任何其他功能。通过SEM，TEM，尺寸分布，CHN分析，FT-IR光谱，显微拉曼光谱，X射线光电子能谱（XPS），ζ电位，能量色散来确认颗粒的形成和修饰的实现。 X射线分析和（EDX）以及热重分析（TGA）证实形成了253±34 nm的颗粒，在0.281 mmol g的载荷下成功完成了巯基在表面的化学注入。^-1。在与As（III）缔合之前和之后，颗粒在水相中显示出适当的分散性和稳定性。As（之间的螯合过程XPS对III）和巯基进行了评估，证实了巯基亚微米清除剂可以最有效地从水中螯合As（III）。评估了可以优化流程的几个因素，例如吸附剂剂量，pH，接触时间，样品量，洗脱液和基质干扰的影响。As（III）校准曲线在0–100μgL ^-1和测定系数之间呈正线性相关（r ² = 0.9981）。在pH = 8.5的条件下，平衡时间为30分钟，可获得最佳的回收率。发现As（III巯基亚微米清除剂中的）取决于洗脱液，在最佳条件下的最大回收率为98±3％。从三个不同的地下水位置中砷（Ⅲ）的平均回收率为97.15％。

更新日期：2017-12-20

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