FLOW-INJECTION FOR THE DETERMINATION OF SE(IV) AND SE(VI) BY HYDRIDE GENERATION ATOMIC-ABSORPTION SPECTROMETRY WITH MICROWAVE-OVEN ONLINE PREREDUCTION OF SE(VI) TO SE(IV)
Jl. Burguera et al., FLOW-INJECTION FOR THE DETERMINATION OF SE(IV) AND SE(VI) BY HYDRIDE GENERATION ATOMIC-ABSORPTION SPECTROMETRY WITH MICROWAVE-OVEN ONLINE PREREDUCTION OF SE(VI) TO SE(IV), Spectrochimica acta, Part B: Atomic spectroscopy, 51(14), 1996, pp. 1837-1847
An on-line flow injection system has been developed for the selective
determination of Se(IV) and Se(VI) in citric fruit juices and geotherm
al waters by hydride generation atomic absorption spectrometry with mi
crowave-aided heating prereduction of Se(VI) to Se(IV). The samples an
d the prereductant solutions (4 mol l(-1) HCl for Se(IV) and 12 mol l(
-1) HCl for Se(VI)) which circulated in a closed-flow circuit were inj
ected by means of a time-based injector. This mixture was displaced by
a carrier solution of 1% v/v of hydrochloric acid through a PTFE coil
located inside the focused microwave oven and mixed downstream with a
borohydride solution to generate the hydride. The linear ranges were
0-120 and 0-100 mu g l(-1) of Se(IV) and Se(VI), respectively. The det
ection limits were 1.0 mu g l(-1) for Se(IV) and 1.5 mu g l(-1) for Se
(VI). The precision (about 2.0-2.5% RSD) and recoveries (96-98% for Se
(IV) and 94-98% for Se(VI)) were good. Total selenium values were also
obtained by electrothermal atomic absorption spectrometry which agree
d with the content of both selenium species. The sample throughput was
about 50 measurements per hour. The main advantage of the method is t
hat the selective determination of Se(IV) and Se(VI) in citric fruit j
uices and geothermal waters is performed in a closed system with a min
imum sample manipulation, exposure to the environment, minimum sample
waste and operator attention.