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用于火焰原子吸收法测定实际样品中痕量 Cd(II)的基于缩水甘油甲基丙烯酸酯的离子印迹聚合物上的 Cd(II)预浓缩的定制材料:多元优化。

Tailored-designed material for the preconcentration of Cd(II) on glycidyl methacrylate-based ion-imprinted polymer for flame atomic absorption for trace determination in real samples: multivariate optimization.

机构信息

Analytical Research Laboratory, Department of Chemistry, Aligarh Muslim University, Aligarh, India, 202002.

出版信息

Environ Sci Pollut Res Int. 2022 Sep;29(45):69068-69081. doi: 10.1007/s11356-022-20558-7. Epub 2022 May 13.

DOI:10.1007/s11356-022-20558-7
PMID:35554830
Abstract

A new Cd(II)-imprinting polymer was synthesised based on glycidyl methacrylate (FeO@GMA@IIP) and employed to develop a dispersive magnetic solid-phase extraction method for the preconcentration prior to the determination of Cd(II) from the environmental samples. A central composite design (CCD) based on response surface methodology was used for optimization of the process variables and the material shows the promising saturation adsorption capacity of 28.21 mg g under the optimum pH of 4.9 within 15.2 min at saturation concentration 914 μg mL. The experimental data were well described by Sips isotherm model and Brouers-Sotolongo fractal kinetic model that indicated the surface heterogeneity and involvement of both chemisorption and physisorption process. Thermodynamic results documented the endothermic and spontaneous nature of adsorption. The sorbent manifest the economic feasibility maintaining its sorption efficiency after the regeneration by 1 M HNO and reusability up to 6 adsorption/desorption cycles. The developed method exhibited the preconcentration factor of 30 and a high degree of tolerance for matrix ions. Limit of detection (LOD) and quantification (LOQ) were calculated as 3.054 and 10.182 μg L respectively. The developed method was validated by the standard reference material and spiking addition method in real samples, and obtained results showed good agreement in accordance with spiking values. The ease of magnetic separation, high selectivity, good adsorption capacity and faster kinetics made this material a promising candidate for Cd(II) determination in various food and aqueous samples.

摘要

一种新型的 Cd(II)印迹聚合物(FeO@GMA@IIP)被合成,并用于开发一种分散磁固相萃取方法,以在环境样品中 Cd(II)的测定之前进行预浓缩。基于响应面法的中心复合设计(CCD)用于优化工艺变量,该材料在最佳 pH 值为 4.9 时表现出有前途的饱和吸附容量为 28.21mg/g,在 15.2min 内达到饱和浓度 914μg/mL。实验数据很好地符合 Sips 等温线模型和 Brouers-Sotolongo 分形动力学模型,表明表面不均匀性和化学吸附和物理吸附过程的参与。热力学结果证明了吸附是吸热和自发的。该吸附剂在 1M HNO 再生后保持其吸附效率,并可重复使用 6 次吸附/解吸循环,表现出经济可行性。所开发的方法表现出 30 的浓缩因子和对基体离子的高容忍度。检测限(LOD)和定量限(LOQ)分别计算为 3.054 和 10.182μg/L。该方法通过标准参考物质和实际样品中的加标回收方法进行了验证,所得结果与加标值吻合良好。该材料易于磁分离、高选择性、良好的吸附容量和较快的动力学,使其成为各种食品和水样中 Cd(II)测定的有前途的候选物。

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