DETERMINATION OF (ULTRA)TRACE AMOUNTS OF ANTIMONY(III) IN WATER BY FLOW-INJECTION ONLINE SORPTION PRECONCENTRATION IN A KNOTTED REACTOR COUPLED WITH ELECTROTHERMAL ATOMIC-ABSORPTION SPECTROMETRY
Xp. Yan et al., DETERMINATION OF (ULTRA)TRACE AMOUNTS OF ANTIMONY(III) IN WATER BY FLOW-INJECTION ONLINE SORPTION PRECONCENTRATION IN A KNOTTED REACTOR COUPLED WITH ELECTROTHERMAL ATOMIC-ABSORPTION SPECTROMETRY, Analyst, 121(8), 1996, pp. 1061-1067
A flow injection on-line sorption preconcentration system has been syn
chronously coupled to an ETAAS system for the selective determination
of (ultra)trace amounts of Sb-III in water, The determination was achi
eved by selective complexation of Sb-III with ammonium pyrrolidine dit
hiocarbamate (APDC) at a wide range of sample acidity (0-1 mol l(-1) H
Cl), sorption of the complex onto the inner walls of a knotted reactor
made from (100 cm long x 0.5 mm id) PTFE tubing, quantitative elution
with 35 mu l of ethanol and subsequent ETAAS detection. In order to m
inimize dispersion and to reduce the eluent volume required for the qu
antitative elution, an air flow was used to drive the eluent elution a
nd to deliver all the eluate into an unpreheated polycrystalline graph
ite tube without a platform, Precise timing was not needed for analyte
elution and eluate introduction, ETAAS determination of the analyte w
as performed in parallel with the preconcentration of the next sample,
Using a preconcentration time of 30 s and a sample loading flow rate
of 5.4 ml min(-1), an enhancement factor of 30 was obtained in compari
son with direct injection of 35 mu l aqueous solution, resulting in a
sampling frequency of 42 samples h(-1). The detection limit (3s) was 0
.021 mu g l(-1) and the precision was 2.9% (RSD) for eleven replicate
determinations at 1 mu g l(-1). The introduction of an efficient wash
step before elution with the addition of APDC to the wash medium permi
tted the use of simple aqueous standards for direct calibration in the
analysis of sea-water. The accuracy of the proposed method was demons
trated by analysing synthetic mixtures and spiked sea-water.