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磁性金属有机骨架(MOF)的合成与表征作为一种新型的吸附剂,并通过实验设计方法对其进行优化,用于环境样品中钯的测定。

Synthesis and characterization of magnetic metal-organic framework (MOF) as a novel sorbent, and its optimization by experimental design methodology for determination of palladium in environmental samples.

机构信息

Department of Chemistry, Shahid Beheshti University, Evin, Tehran, Iran.

出版信息

Talanta. 2012 Sep 15;99:132-9. doi: 10.1016/j.talanta.2012.05.030. Epub 2012 May 26.

Abstract

This paper describes the synthesis and application of novel magnetic metal-organic framework (MOF) [(Fe(3)O(4)-Pyridine)/Cu(3)(BTC)(2)] for preconcentration of Pd(II) and its determination by flame atomic absorption spectrometry (FAAS). A Box-Behnken design was used to find the optimum conditions for the preconcentration procedure through response surface methodology. Three variables including amount of magnetic MOF, extraction time, and pH of extraction were selected as factors for adsorption step, and in desorption step, four parameters including type, volume, and concentration of eluent, and desorption time were selected in the optimization study. These values were 30 mg, 6 min, 6.9, K(2)SO(4)+NaOH, 6 mL, 9.5 (w/v %)+0.01 mol L(-1), 15.5 min, for amount of MOF, extraction time, pH of extraction, type, volume, and concentration of the eluent, and desorption time, respectively. The preconcentration factor (PF), relative standard deviation (RSD), limit of detection (LOD), and adsorption capacity of the method were found to be 208, 2.1%, 0.37 ng mL(-1), and 105.1 mg g(-1), respectively. It was found that the magnetic MOF has more capacity compared to Fe(3)O(4)-Py. Finally, the magnetic MOF was successfully applied for rapid extraction of trace amounts of Pd (II) ions in fish, sediment, soil, and water samples.

摘要

本文描述了新型磁性金属-有机骨架[(Fe(3)O(4)-吡啶)/Cu(3)(BTC)(2)]的合成及其在 Pd(II)的预浓缩及其火焰原子吸收光谱法(FAAS)测定中的应用。通过响应面法,使用 Box-Behnken 设计寻找预浓缩过程的最佳条件。三个变量,包括磁性 MOF 的量、萃取时间和萃取 pH 值,被选为吸附步骤的因素,而在解吸步骤中,四种参数,包括洗脱液的类型、体积和浓度以及解吸时间,在优化研究中被选择。这些值分别为 30mg、6min、6.9、K(2)SO(4)+NaOH、6mL、9.5(w/v %)+0.01mol L(-1)、15.5min,用于 MOF 的量、萃取时间、萃取 pH 值、洗脱液的类型、体积和浓度以及解吸时间。该方法的预浓缩因子(PF)、相对标准偏差(RSD)、检测限(LOD)和吸附容量分别为 208、2.1%、0.37ng mL(-1)和 105.1mg g(-1)。结果表明,与 Fe(3)O(4)-Py 相比,磁性 MOF 具有更高的容量。最后,该磁性 MOF 成功应用于快速提取鱼类、沉积物、土壤和水样中痕量 Pd(II)离子。

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