We report here a highly selective enzymeless approach for the determination of phosphate (PO(4)(3-)) by flow injection analysis (FIA). In this system, the activation of barrel plated nickel electrode (Ni-BPE) in alkaline media to form a Ni(OH)(2)/NiO(OH) film was found to trigger the adsorption of phosphate at the electrode surface. Based on the suppressed current of the electrocatalytic oxidation of glucose at the activated Ni-BPE in 0.1 M NaOH solution caused by adsorption of phosphate, we develop an FIA detection scheme for the determination of phosphate. Under the optimized conditions of flow rate = 300 microL/min and detection potential = 0.55 V vs Ag/AgCl with 25 microM glucose in 0.1 M NaOH as carrier solution, the calibration curve showed a linear range up to 1 mM. Possible interferences from the coexisting ions were also investigated. The results demonstrated that sensor could be used for the determination of phosphate in the presence of nitrate, chloride, sulfate, acetate, oxalate, carbonate, and some anionic species of toxicological and environmental interest, such as chlorate, chromate, and arsenate ions. The electrode can be effectively regenerated without extra treatment under the hydrodynamic condition. For eight continuous injections of 40 microM PO(4)(3-), a relative standard deviation of 0.28% was obtained, indicating good reproducibility of the proposed method. The detection limit (S/N = 3) was calculated as 0.3 microM.
A simple electrochemical approach, which does not require any expensive and complex instruments, is established for the selective and quantitative recognition of melamine in diary products and pet foods. During a preconcentration step (at 1.8 V versus Ag/AgCl), the formation of a polymer film from melamine on a preanodized screen-printed carbon electrode was identified by SEM and XPS. The as-formed polymer was found to be electroactive with a reversible redox peak, and hence square-wave voltammetry was applied to further increase the detection sensitivity to meet the detection limit for application in real sample analysis. Simply with a medium exchange procedure, melamine was selectively detected with a detection limit (S/N=3) of 0.8 μM (i.e., 98.3 ppb) by square-wave voltammetry. Lower than 1 ppm of melamine in real samples can be easily detected with good recoveries of 98.7-100.9% by the proposed approach. The recovery tests established for external calibration and standard addition techniques verified that the analysis can be done in a single-run measurement.
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