首页> 外文期刊>Journal of the Brazilian Chemical Society >Synthesis of Nano-Pore Size Ag(I)-Imprinted Polymer for the Extraction and Preconcentration of Silver Ions Followed by Its Determination with Flame Atomic Absorption Spectrometry and Spectrophotometry Using Localized Surface Plasmon Resonance Peak of Silver Nanoparticles
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Synthesis of Nano-Pore Size Ag(I)-Imprinted Polymer for the Extraction and Preconcentration of Silver Ions Followed by Its Determination with Flame Atomic Absorption Spectrometry and Spectrophotometry Using Localized Surface Plasmon Resonance Peak of Silver Nanoparticles

机译:纳米孔大小的Ag(I)印迹聚合物的合成,用于银离子的提取和预富集,然后通过火焰原子吸收光谱法和分光光度法使用银纳米粒子的局部表面等离子体共振峰进行测定

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Silver ion imprinted polymer (IIP) was synthesized in the presence of Ag(I)-N,N’‑bis(salicylidene)ethylenediamine (salen) complex using 4-vinylpyridine as the functional monomer, ethylene glycol dimethacrylate (EGDMA) as the crosslinker, and 2,2-azobis(isobutyronitrile) (AIBN) as the initiator. The Ag(I)-imprinted polymer (IIP) particles were characterized by SEM (scanning electron microscope), FTIR (Fourier transform infrared spectroscopy) and BET/BJH (Brunauer-Emmett-Teller/Barrett-Joyner-Halenda) analysis. The imprinted Ag(I) ions were completely removed by leaching the IIP with thiourea (0.5 mol L-1). The polymer was employed as a selective sorbent for extraction and separation of the trace amounts of the Ag(I) ions. The preconcentrated ion was determined via the flame atomic absorption spectrometry (FAAS) or it was reduced to silver nanoparticles and quantified by spectrophotometry based on its localized surface plasmon resonance peak (LSPRP). The figures of merit of both methods were compared. Under the optimized conditions, a sample volume of 80 mL resulted in an enhancement factor of 312. The detection limit (3Sb/m) and the relative standard deviation (n = 10) at 10 µg L-1 level for FAAS were found to be 0.06 µg L-1, 2.9%, whereas for the LSPRP method they were 0.5 µg L-1 and 10.3%, respectively. The methods were successfully applied to the determination of silver in radiology film, hair, nails, and water samples.
机译:银离子印迹聚合物(IIP)是在Ag(I)-N,N'-双(水杨基亚乙基)乙二胺(salen)络合物的存在下合成的,使用4-乙烯基吡啶作为功能单体,乙二醇二甲基丙烯酸酯(EGDMA)作为交联剂和2,2-偶氮二(异丁腈)(AIBN)作为引发剂。通过SEM(扫描电子显微镜),FTIR(傅立叶变换红外光谱)和BET / BJH(Brunauer-Emmett-Teller / Barrett-Joyner-Halenda)分析对Ag(I)印迹聚合物(IIP)颗粒进行表征。通过用硫脲(0.5 mol L-1)浸出IIP,可以完全除去印迹的Ag(I)离子。该聚合物用作选择性吸附剂,用于萃取和分离痕量的Ag(I)离子。通过火焰原子吸收光谱法(FAAS)确定预浓缩离子,或将其还原为银纳米颗粒,并基于其局部表面等离子体共振峰(LSPRP)通过分光光度法对其进行定量。比较了两种方法的优值。在最佳条件下,样品体积为80 mL,增强因子为312。FAAS的检出限(3Sb / m)和相对标准偏差(n = 10)在10 µg L-1处为0.06 µg L-1,2.9%,而对于LSPRP方法,分别为0.5 µg L-1和10.3%。该方法已成功应用于放射线胶片,头发,指甲和水样中银的测定。

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