Abstract: | Dithizone (diphenylthiocarbazone) dissolved in chloroform was employed as a ligand for the solvent extraction of either cadmium or zinc from aqueous media. Acoustic emulsification was shown to be effective both in extraction and recovery or ‘back extraction’ with a fresh clean aqueous solution. Quantitative analysis of cadmium or zinc removed via double sono‐extraction from aqueous media hostile to voltammetric analysis proceeded via sono‐square wave anodic stripping voltammetry (sono‐SWASV), resulting in high sensitivity in the relatively clean medium. This technique was shown to be viable for the quantification of cadmium from surfactant containing media where direct electroanalytical techniques fail. The method was also applied to the analysis of zinc in commercial shampoo and toothpaste, giving results in close agreement with those obtained from independent analysis. Biphasic sono‐extraction synergistically coupled with sono‐SWASV therefore presents an attractive technique for cadmium or zinc analysis in electrode passsivating media. The technique likely removes contaminants present in the test solution since these will ‘prefer’ to remain in the initial aqueous phase, or will transfer to the extracting organic phase, but are unlikely to be doubly transferred into the clean final aqueous phase. |