Determination of bismuth in aluminium and in steels by electrothermal atomic absorption spectrometry after on-line separation using a minicolumn of activated carbon
Jbb. Da Silva et al., Determination of bismuth in aluminium and in steels by electrothermal atomic absorption spectrometry after on-line separation using a minicolumn of activated carbon, ANALYST, 124(8), 1999, pp. 1249-1253
A simple on-line separation and preconcentration flow injection system for
the determination of Bi in steels and aluminium solutions by electrothermal
atomic absorption spectrometry is proposed. The system requires only a man
ual injector-commutator and a peristaltic pump. Bismuth is separated after
complexation with the ammonium salt of dithiophosphoric acid O,O-diethyl es
ter and sorption in a minicolumn filled with activated carbon, using ethano
l as eluent, which is received in the autosampler cup of the electrothermal
atomic absorption spectrometer. A L'vov platform covered with 500 mu g of
Ir allows a pyrolysis temperature of 900 degrees C. The preconcentration, p
re-elution and elution flow rates were optimized. The column was cleaned wi
th 2 mL of ethanol followed by 5 mL of water. For 10 mL of sample solution,
an enrichment factor of about 14 was obtained for Bi in Al or Fe matrices.
The detection limit, in the sample solution, was 0.048 mu g L-1. The linea
r regression coefficients of the calibration curves were better than 0.997.
For the certified steel samples, the results were in agreement with the re
ference values. For the non-certified aluminium sample, the recoveries of s
piked samples were in the range 87-105%. The fact that the complexing agent
does not complex Al and Fe(II) allows the separation of more than 99.5% of
the major components.