Journal
MICROCHIMICA ACTA
Volume 150, Issue 1, Pages 59-65Publisher
SPRINGER WIEN
DOI: 10.1007/s00604-005-0333-8
Keywords
solvent sublation; dithizone; trace elements; water
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Solvent sublation was studied as a method of separating and pre-concentrating traces of Zn(II), Cd(II) and Cu(II) as diphenylthiocarbazone (dithizone) complexes for their determination. The experimental conditions, such as pH of solution, amount of dithizone as ligand, stirring time, gas flow rate and flotation time, were optimized. Different non-ionic surfactants and types of organic solvents were optimized for efficient sublation. The analyte ions in a 350mL sample were complexed as metal-dithizone complexes by adding 10mL of 0.084% dithizone, 0.5mL of 0.1% nonylphenol polyoxyethylene ether (NP) and 10mL of pH 4.3 potassium hydrogen phthalate-sodium hydroxide buffer solution. The solution was stirred with a mechanical stirrer for 30 min. It was transferred to a flotation cell, and the complexes were floated by bubbling air and extracted into 10mL of methylisobutyl ketone (MIBK) on the surface of the aqueous solution. The analytes in the organic phase were determined by flame atomic absorption spectrometry ( F-AAS) for Zn( II) and by graphite furnace atomic absorption spectrometry (GF-AAS) for Cd( II) and Cu( II). The proposed method was applied to determine Zn( II), Cd( II) and Cu( II) in real water samples; the enrichment factor was more than 37, the RSD was less than 4.26%, recoveries ranged from 92.7 to 107.3%, and the detection limits were 1.0 mgL(-1) for Zn(II), 0.006 mgL(-1) for Cd(II) and 0.06 mgL(-1) for Cu(II). The results obtained were satisfactory.
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