Adsorption and deposition-assisted anodic stripping voltammetry for determination of antimony(III) in presence of hematoxylin on glassy carbon electrode.

A validated simple, reliable and sensitive adsorptive anodic stripping voltammetric procedure is suggested for the accurate determination of antimony(III) on a glassy carbon electrode (GCE) in the presence of hematoxylin (HT), used as a chemical receptor in antimony analysis for the first time. Under optimized conditions, the plot of stripping peak current versus Sb(III) concentration showed two dynamic linear ranges, 1.0×10-4 - 0.01µm (R2 =0.9986) and 0.01 - 1.0µm (R2 =0.9973) with a detection limit of 9.5×10-11molL-1 (11.57ngL-1). The RSD values of intra-day precision and inter-day precision (n =5) for 5.0×10-7molL-1 Sb(III) were calculated as 1.63% and 2.27%, respectively, indicating that the proposed method has a good precision. Recoveries for Sb(III) in water samples were found to be between 97% and 102% for the 5.0×10-7molL-1 Sb(III), proving the reliability and accuracy of the method proposed.

Electrocatalytic oxidation of NADH using a pencil graphite electrode modified with quercetin.

In the present study, the electrocatalytic oxidation of reduced ß nicotinamide adenine dinucleotide (NADH) was investigated using a pencil graphite electrode modified with quercetin (PGE/QH(2)). The PGE/QH(2) was prepared through two steps: (i) the pre-treatment of PGE at 1.40 V vs. Ag|AgCl|KCl((sat.)) in pH 7.0 phosphate buffer containing 0.1 M KCl for 60s and (ii) adsorption of QH(2) on the PGE via immersion of PGE into a 1.0mM QH(2) solution (in ethanol) for 60s. Cyclic voltammetric studies show that the peak potential of NADH oxidation shifts from +500 mV at bare PGE to +300 mV at PGE/QH(2). The electrocatalytic currents obtained from amperometric measurements at +300 mV vs. Ag|AgCl|KCl((sat.)) and in phosphate buffer solution at pH 7.0 containing 0.1M KCl were linearly related to the concentration of NADH. Linear calibration plots are obtained in the concentration range from 0.5 µM to 100 µM. The limit of detection was found to be 0.15 µM.

Photoelectrocatalytic oxidation of NADH in a flow injection analysis system using a poly-hematoxylin modified glassy carbon electrode.

A stable electroactive thin film of poly-hematoxylin (poly-HT) was successfully prepared on a glassy carbon electrode (GCE) surface by recording successive cyclic voltammograms of 0.3 mM HT, in a phosphate buffer solution (pH 7.0) containing 0.1 M NaNO3, in the potential range of -0.5 to +2.0 V vs. Ag/AgCl. The deposition of HT on GCE surface can be explained through the electropolymerization process. This poly-HT modified electrode exhibited a good electrocatalytic activity towards the NADH oxidation in a phosphate buffer solution (pH 7.0), and led to a significant decrease in the overpotential by more than 320 mV compared with the bare GCE. In order to perform the photoelectrocatalytic determination of NADH in a flow injection analysis (FIA) system, a home-made flow electrochemical cell with a suitable transparent window for irradiation of the electrode surface was constructed. Flow rate of carrier solution, transmission tubing length, injection volume and applied potential for the amperometric and photoamperometric FIA studies were optimized as 1.3 mL min(-1), 10 cm, 100 µL and +300 mV vs. Ag/AgCl, respectively. The currents obtained from amperometric and photoamperometric measurements in FIA system at optimum conditions were linearly dependent on the NADH concentration and linear calibration curves were obtained in the range of 1.0×10(-7)-1.5×10(-4) M and in the range of 1.0×10(-7)-2.5×10(-4) M NADH, respectively. The relative standard deviation (RSD) of six replicate injections of 6.0×10(-5) M NADH was calculated as 2.2% and 4.3% for the amperometric and the photoamperometric method, respectively. The limit of detection was found to be 3.0×10(-8) M for the photoamperometric determination of NADH.