A simple and efficient method for the selective separation and preconcentration of Ag+ using homogeneous liquid-liquid extraction was developed. Tetraspirocyclohexylcalix[4]pyrrole (TSCC4P) was synthesized and investigated as a suitable selective complexing ligand for Ag+. Zonyl FSA (FSA) was applied as a phase-separator agent under mild pH conditions. Under the optimal conditions ([TSCC4P] = 3.4 x 10(-4) M, [THF] = 25.0% v/v, [FSA] = 1.25% w/v, and pH = 4.5), 5 microg of Ag+ in 6.0 ml aqueous phase could be extracted quantitatively into 20 microl of the sedimented phase. The maximum concentration factor was 300-fold. The limit of detection of the proposed method was 0.005 ng/ml. The reproducibility of the proposed method was at most 3.5%. The influence of the pH, type and volume of the water-miscible organic solvent, concentration of FSA, concentration of the complexing ligand and the effect of different diverse ions on the extraction and determination of Ag+ were investigated. The proposed method was applied to the extraction and determination of Ag+ in different water samples.
An efficient one-pot quantitative procedure for the preparation of functionalized benzo[a]pyrano[2,3-c]phenazine derivatives from four-component reaction of 2-hydroxynaphthalene-1,4-dione, o-phenylenediamine, aldehydes, and malononitrile in the presence of nano CuO as the catalyst has been developed. The copper(II) oxide nanoparticles can be recovered and reused several times without loss of its activity.
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