Abstract

• Pyrrole-1-carboxylic acid (Py-CO 2 ) was synthesized and applied for modification of pencil graphite electrodes (PGE). • Electropolymerization of Py-CO 2 created a sensing film for selective metal extraction and determination. • The modified electrode, PPy-CO 2 @PGE, provided excellent sensitivity and selectivity for detection of Pb 2+ and Cd 2+ . • Accurate analysis of Pb 2+ and Cd 2+ in several natural water sources was demonstrated and independently verified. A pencil graphite electrode (PGE) was modified by the electropolymerization of pyrrole-1-carboxylic acid (Py-CO 2 ) to form a sensing film of poly(pyrrole-1-carboxylic acid) (PPy-CO 2 ) for the sensitive determination of Pb 2+ and Cd 2+ by differential pulse anodic stripping voltammetry (DPASV). The porous structure of the PPy-CO 2 film uniformly distributes a carboxylate group throughout the coating to selectively coordinate and preconcentrate metal ions. The polymer film was characterized by cyclic voltammetry (CV), scanning electron microscopy (SEM), and energy dispersive X-ray (EDS) and Fourier transform infrared (FTIR) spectroscopy. Under the optimized conditions (analyte solution pH: 6.0, extraction time: 15 min, reduction potential: −1.1 V and reduction time: 160 s), a linear relationship between peak current and metal concentration was obtained from 0.1 to 1 nM for Pb 2+ and Cd 2+ with detection limits of 0.018 and 0.023 nM, respectively. Simultaneous analysis of Pb 2+ and Cd 2+ was performed in the presence of the possible interfering ions Cr 3+ , Bi 3+ , Cu 2+ , Fe 2+ , Zn 2+ and Co 2+ and in complex matrices. The performance of the PPy-CO 2 @PGE demonstrated excellent intra-day repeatability, long-term reproducibility over a seven-week period and was utilized for the determination of Pb 2+ and Cd 2+ in a variety of natural water samples with the results independently verified by inductively coupled plasma-mass spectrometry.

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