This paper describes the preparation and electrochemical application of a new chemically modified electrode for simple and highly sensitive simultaneous determination of copper, mercury and cadmium using cyclic voltammetry (CV) and differential pulse voltammetry (DPV). Firstly, a new bis‐Schiff base ligand, 2,2′‐((pyridine‐2,6‐diylbis (azanylylidene)) bis (methanylylidene))bis(4‐bromophenol) (ligand L) has been synthesized by reaction of the 2,6‐diamino pyridine with 5‐bromo salicylaldehyde or salicylaldehyde at ethanol under refluxing. The structure of the synthesized compound resulted from the IR, 1HNMR, MS, UV spectroscopy and elemental analysis data. Afterwards, a novel, simple and effective chemically modified carbon paste electrode with ligand L was prepared. The electrochemical properties and applications of the modified electrode, including the pH, percentage of modifier, the electron transfer, optimized conditions, linear response and detection limit were investigated. High sensitivity and reproducibility, together with the ease of preparation and regeneration of the electrode surface by simple polishing, make the electrode very suitable for the voltammetric determination of copper, mercury and cadmium in several Merck samples and water samples.
In this research, solvent-assisted dispersive micro-SPE was introduced as a simple modified technique for the determination of parabens in water and cosmetic samples. Aminopropyl-functionalized magnetite nanoparticles (MNPs) were successfully synthesized and applied. GC with photoionization detector was used for the separation and detection of parabens. In this method, hexylacetate (15 μL) as a solvent and aminopropyl-functionalized MNPs (5 μg) as a sorbent were added to an aqueous sample (10 mL) and then the sample was sonicated. Dispersed magnetite was collected in the bottom of the conical tube by using a strong magnet and then ACN was added as a desorption solvent. Forty microliters of this solvent was transferred into a microvial and then acetic anhydride and pyridine were added, thus derivatization was performed by acetic anhydride. After evaporation, 1 μL of derivatized sample was injected into a gas chromatograph for analysis. Several important parameters, such as kind of organic solvent, desorption solvent and volume, amount of aminopropyl-functionalized MNPs and effect of salt addition were investigated. Under optimum conditions, the limits of detection achieved were between 50 and 300 ng/L, with RSDs (n = 5) lower than 8%. Under the optimum conditions, the enrichment factors ranged from 217 to 1253 and the extraction recoveries ranged from 10 to 62%. The recoveries were obtained for the analytes in river water and mouthwash solution and hand cream in the range of 87-103%. The advantages of proposed method are simplicity of operation, rapidity, high extraction yields, and environmental friendly character.
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