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A disposable electrochemical sensor based on bifunctional periodic mesoporous organosilica for the determination of lead in drinking waters

机译:一种基于双功能周期性介孔有机硅的一次性电化学传感器,用于测定饮用水中的铅

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A new bifunctional disulfide-and tetrasulfide-bridged periodic mesoporous organosilica (PMO) with mercaptothiazoline ligand was synthesized and employed to prepare chemically modified carbon paste electrodes for Pb(II) detection in aqueous media by square wave adsorptive stripping voltammetry. To demonstrate the real interest of bifunctionalization, carbon paste electrodes were prepared with disulfide-and tetrasulfide-bridged PMO without mercaptothiazoline ligand. Results showed the importance of bifunctionalization of PMOs to improve the sensitivity for the determination of Pb(II) in water samples. To achieve the most accurate and sensitive Pb(II) measurements, optimization of the operating parameters in preconcentration and detection steps was performed. Finally, the modified carbon paste electrode prepared with bifunctional disulfide-bridged PMO with mercaptothiazoline ligand was applied to determine Pb(II) in different water samples without any pretreatment. Using this electrode, the optimal operating conditions were 120 s of electrolysis time in HCl 0.4 M. In these conditions, the voltammetric signal increased linearly with the preconcentration time from 1 to 10 min. Under optimized conditions, the linear range was 2-100 mu g/ L (R-2= 0.9943) with a detection limit of 0.5 mu g/L (for 5-min preconcentration time). Good reproducibility was achieved on both single and equally prepared electrodes. The accuracy of the method was validated by analysing Pb(II) in different drinking and natural water samples, with spiked recoveries in the range of 95-105 +/- 10 %. The results demonstrated that the prepared electrochemical sensor exhibited selectivity, fast response time and exceptional long-time stability.
机译:合成了具有巯基噻唑啉配体的新型双功能二硫键和四硫键桥接的周期性介孔有机硅(PMO),并通过方波吸附溶出伏安法制备了用于水介质中Pb(II)检测的化学修饰碳糊电极。为了证明双功能化的真正意义,碳糊电极是用不带巯基噻唑啉配体的二硫键和四硫键桥接的PMO制备的。结果表明,将PMO进行双功能化对于提高测定水样中Pb(II)的敏感性非常重要。为了实现最准确和最灵敏的Pb(II)测量,在预浓缩和检测步骤中对操作参数进行了优化。最后,将未经修饰的碳糊电极用双功能二硫桥联的PMO和巯基噻唑啉配体制备,用于测定不同水样中的Pb(II)。使用此电极,最佳操作条件是在0.4 M的HCl中电解时间为120 s。在这些条件下,伏安信号随预浓缩时间从1分钟到10分钟呈线性增加。在优化条件下,线性范围为2-100μg / L(R-2 = 0.9943),检测极限为0.5μg / L(5分钟预浓缩时间)。在单个电极和同样准备的电极上均实现了良好的重现性。通过分析不同饮用水和天然水样品中的Pb(II)验证了该方法的准确性,加标回收率在95-105 +/- 10%的范围内。结果表明,所制备的电化学传感器具有选择性,快速响应时间和出色的长期稳定性。

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