Analytical Sciences

Determination of Silver(I) by Electrothermal-AAS in a Microdroplet Formed from a Homogeneous Liquid-Liquid Extraction System Using Tetraspirocyclohexylcalix[4]pyrroles

Ali Reza GHIASVAND,* Farzaneh MORADI,* Hashem SHARGHI,** and Ali Reza HASANINEJAD**

*Department of Chemistry, Lorestan University, Khorram-Abad, Iran
**Department of Chemistry, Shiraz University, Shiraz, Iran

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 × 10^-4 M, [THF] = 25.0% v/v, [FSA] = 1.25% w/v, and pH = 4.5), 5 µg of Ag⁺ in 6.0 ml aqueous phase could be extracted quantitatively into 20 µl 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.

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