H. Ono et al., SIMULTANEOUS DETERMINATION OF COPPER, SIL VER AND CADMIUM IN HIGH-PURITY ZINC BY ICP-AES AFTER EXTRACTION AND BACK-EXTRACTION, Bunseki Kagaku, 46(2), 1997, pp. 153-158
The separation and simultaneous determination of trace amounts of Cu,
Ag, and Cd in high-purity Zn were studied. After the sample was dissol
ved in a mixture of sulfuric acid and nitric acid, Cu, Pig and Cd were
separated from Zn by extraction into xylene as diethyldithiocarbamate
s complexes using diethylammonium diethyldithiocarbamate (DDDC), and t
hen back-extracted into nitric acid for a determination by ICP-AES. Th
e recoveries of Cu, Ag and Cd were satisfactory throughout the extract
ion with 2.5x10(-2) mol/l DDDC in xylene from 0.25 mol/l sulfuric acid
-0.1 mol/l nitric acid solution and the back-extraction with 7.5 mol/l
nitric acid. The extractions of Cu, Ag and Cd were suppresed in the p
resence of hydrochloric acid. The diverse elements in Zn caused no int
erference for the determination of Cu, Ag and Cd. The recoveries of Cu
, Ag and Cd decreased somewhat with increasing the added amount of Zn.
Thus, the standard addition method should be applied for the determin
ation of these metals. The detection limits were found to be 0.17 mu g
/g for Cu, 0.12 mu g/g for Ag and 0.07 mu g/g for Cd using 1 g of a Zn
sample. The proposed method was applied to an analysis of the referen
ce material, the results agreed with the certified values.