Molybdenum determination in iron matrices by ICP-AES after separation and preconcentration using polyurethane foam.
A procedure is proposed for the separation and determination of molybdenum in iron matrices by a batch process. It is based on the solid-phase extraction of the molybdenum(V) ion as thiocyanate complex on polyurethane (PU) foam. The extraction parameters were optimized. Using 0.20 mol L-1 hydrochloric acid, a thiocyanate concentration of 0.10 mol L-1, 100 mg of polyurethane foam and shaking time of 10 min, molybdenum (5-400 micrograms) can be separated and preconcentrated from large amounts of iron (10 mg). Desorption was carried out instantaneously by conc. nitric acid or acetone. Distribution coefficients, sorption capacity of the PU foam and coefficients of variation were also evaluated. The effect of some ions on the separation procedure was assessed. Iron(III) should be reduced to iron(II). The proposed procedure was used to determine molybdenum in standard iron matrices such as steel and pure iron. The achieved results did not show significant differences with certified values.
Ferreira
S L
SL
Universidade Federal da Bahia, Instituto de Química, Salvador, Bahia, Brasil 40170-290. slcf@ufba.br
dos Santos
H C
HC
de Jesus
D S
DS