Küçüksakalli Melike, Salamat Qamar, Tireli Buket, Elçi Şükrü Gökhan
Department of Biomedical Engineering, Faculty of Technology, Pamukkale University, Denizli, Turkiye.
Turk J Chem. 2024 Jul 14;48(4):620-630. doi: 10.55730/1300-0527.3683. eCollection 2024.
A novel FeO@coPPy-PTH nanocomposite-based sorbent was prepared via in situ oxidative polymerization using FeO nanoparticles with spherical and flower-like morphologies of thiophene and pyrrole as the feedstocks. The synthesized nanocomposite displayed sensitive extraction and determination of metal ions Co(II), Cr(III), and Ni(II) without a chelating agent, followed by microsample injection system-flame atomic absorption spectrometry. Advanced spectroscopic and imaging techniques including scanning electron microscopy (SEM) and Fourier transform infrared spectroscopy were used to characterize the composition and morphology of the FeO@coPPy-PTH nanocomposite. SEM observations showed that the size of the FeO nanoparticles changed from 30 nm to 120 nm in diameter after copolymer (PPy-PTH) coating. The FeO@coPPy-PTH nanocomposite has good dispersion properties and stability in strong acid solutions. For effective extraction of the studied analytes, the influence of sample pH, volume of sample solution and eluent, amount of adsorbent, and interference of coexisting metal ions were optimized. Under the optimum conditions, preconcentration factors were obtained as 25 for all analytes. The calibration curves were linear in the range of 0.0-10.0 μg L with coefficients of determination (R) greater than 0.9957 for all three analytes. Limits of detection (S/N = 3) were calculated in the range of 0.17-0.23 μg L. Precision values, expressed as relative standard deviations, were lower than 3.0%, and relative recoveries were obtained in the range of 88.6%-103.6%. The proposed method (FeO@coPPy-PTH/MSPE/MIS-FAAS) was successfully applied to extract and determine the studied metal ions in beer, wine, and nonalcoholic beverage samples.
通过原位氧化聚合,以具有球形和花状形态的FeO纳米颗粒、噻吩和吡咯为原料,制备了一种新型的基于FeO@coPPy - PTH纳米复合材料的吸附剂。合成的纳米复合材料在无需螯合剂的情况下,对金属离子Co(II)、Cr(III)和Ni(II)表现出灵敏的萃取和测定能力,随后采用微量进样系统 - 火焰原子吸收光谱法进行检测。利用包括扫描电子显微镜(SEM)和傅里叶变换红外光谱在内的先进光谱和成像技术对FeO@coPPy - PTH纳米复合材料的组成和形态进行了表征。SEM观察表明,共聚物(PPy - PTH)包覆后,FeO纳米颗粒的直径从30 nm变为120 nm。FeO@coPPy - PTH纳米复合材料在强酸溶液中具有良好的分散性能和稳定性。为了有效萃取所研究的分析物,对样品pH值、样品溶液和洗脱液体积、吸附剂用量以及共存金属离子的干扰进行了优化。在最佳条件下,所有分析物的预富集因子均为25。校准曲线在0.0 - 10.0 μg/L范围内呈线性,三种分析物的测定系数(R)均大于0.9957。检测限(S/N = 3)在0.17 - 0.23 μg/L范围内计算得出。以相对标准偏差表示的精密度值低于3.0%,相对回收率在88.6% - 103.6%范围内。所提出的方法(FeO@coPPy - PTH/MSPE/MIS - FAAS)成功应用于啤酒、葡萄酒和非酒精饮料样品中所研究金属离子的萃取和测定。