Synergic extraction of zinc, cadmium and lead with hexafluoroacetylacetone and di-n-butylsulphoxide and tri-n-butyl phosphate, and the gas chromatography of the zinc adduct.
The synergic solvent extraction of zinc(II), cadmium(II), and lead(II) with 1,1,1,5,5,5-hexafluoro-2,4-pentanedione, H(HFA), and tri-n-butyl phosphate (TBP) or di-n-butylsulphoxide (DBSO) as neutral donors, into cyclohexane has been investigated. Quantitative extraction occurs at pH 4.5-6.0 in extraction times of 10-30 min, depending on the metal species. The optimum pH, equilibration time, stoichiometry and stability of the extracted species, as well as the effect of fluorinated beta-diketone concentration, metal concentration and neutral donor concentration on the extraction are reported. The extracted species was found to be M(HFA)(2).2DBSO or M(HFA)(2).2TBP by mass-action studies. Thermogravimetric analysis of the complexes is reported. The gas chromatographic behaviour of the ternary complexes of the three metals has also been studied. A calibration plot of peak area vs. the amount of zinc injected was linear over the range 40-900 ng of zinc for the Zn(HFA)(2). 2DBSO species; the cadmium and lead species apparently decomposed on the column and useful chromatographic peaks were not observed. The calibration plot for zinc was determined on the basis of the averages of 3-5 replicate determinations for 14 different concentrations over the range stated. The average relative standard deviation was 2.9%.
O'Laughlin
J W
JW
Department of Chemistry, University of Missouri, Columbia, Missouri 65201, USA.
O'Brien
T P
TP